CN112755955A - Preparation method of light honeycomb molecular sieve purification module - Google Patents
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- CN112755955A CN112755955A CN202011573130.6A CN202011573130A CN112755955A CN 112755955 A CN112755955 A CN 112755955A CN 202011573130 A CN202011573130 A CN 202011573130A CN 112755955 A CN112755955 A CN 112755955A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/2803—Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products
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- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28042—Shaped bodies; Monolithic structures
- B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
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- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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Abstract
The embodiment of the invention discloses a preparation method of a light honeycomb molecular sieve purification module, which comprises the following steps: a sample initial mixing step: putting the weighed molecular sieve raw powder, the binder and the foaming agent into a mixer, and stirring and mixing the materials uniformly; a sample pugging step: adding the weighed surfactant, continuously stirring, and putting the mud-shaped blank into a mud mill for extrusion; an extrusion molding step: putting the smelted pug into a low-pressure vacuum extruder for molding and extruding; and (3) low-temperature drying: placing the wet green body in a low-temperature drying environment; and (3) low-temperature foaming step: foaming the wet green body at low temperature; and (3) calcining: and (3) calcining the blank at high temperature to obtain the light honeycomb molecular sieve. According to the invention, more hollow structures are obtained by artificially controlling foaming and pore-forming, so that the overall density of the honeycomb molecular sieve is reduced, the specific surface area of a honeycomb molecular sieve module is increased, contact adsorption of waste gas components and the honeycomb molecular sieve is facilitated, and the unit effective adsorption capacity is improved.
Description
Technical Field
The invention relates to the technical field of environmental protection, in particular to a preparation method of a light honeycomb molecular sieve purification module.
Background
Molecular sieves have found wide application in the fields of catalysis, adsorption and the like due to their advantages of thermal stability, acid resistance, excellent selectivity and the like. However, the traditional molecular sieve is mainly in powder or granular form, so that the application field and the application range of the traditional molecular sieve are greatly limited, and especially in the field of environmental protection treatment, the granular molecular sieve has large filling resistance and restricts the application of material engineering.
The honeycomb material is a breakthrough of a molecular sieve applied in the field of environmental protection, and has the advantages of good permeability, low resistance, convenient filling, good mechanical strength and the like. But also has the defects that compared with the honeycomb activated carbon with the same volume, the honeycomb activated carbon has the problems of low adsorption capacity, large stacking density and high price, and has great influence on the replacement of the honeycomb activated carbon by the honeycomb molecular sieve in the environmental protection engineering.
Therefore, the effective adsorption capacity of the unit volume of the honeycomb molecular sieve is increased, the stacking density of the honeycomb molecular sieve is reduced, the material utilization rate is improved, the cost is reduced, and the method becomes an important breakthrough for promoting the application of the honeycomb molecular sieve.
Disclosure of Invention
The technical problem to be solved by the embodiment of the invention is to provide a preparation method of a light honeycomb molecular sieve purification module so as to obtain more molecular sieve contact areas and improve the effective adsorption capacity per unit.
In order to solve the technical problem, an embodiment of the present invention provides a preparation method of a light honeycomb molecular sieve purification module, including:
a sample initial mixing step: weighing the following raw materials in percentage by weight: 60-80% of molecular sieve raw powder, 25-15% of binder, 10-3% of surfactant and 5-2% of foaming agent; putting the weighed molecular sieve raw powder, a binder and a foaming agent into a mixer, stirring and mixing the materials uniformly, wherein the binder is clay;
a sample pugging step: adding the weighed surfactant, continuously stirring, putting the uniformly stirred mud-shaped blank into a mud mill, repeatedly mixing and extruding to obtain the well-mixed mud material, and controlling the temperature of the mud material to be
Coarse smelting is repeated for 5 times, and vacuum degree is
An extrusion molding step: putting the smelted pug into a low-pressure vacuum extruder for molding and extruding to obtain a wet blank;
and (3) low-temperature drying: placing the wet green body in a low-temperature drying environment, drying to remove excessive water, and reducing the water content of the wet green body to 18%;
and (3) low-temperature foaming step: foaming the wet blank at a low temperature of 80-90 ℃ for 24h, and naturally cooling to room temperature to obtain a blank containing a naturally air-dried foam;
and (3) calcining: and (3) calcining the blank at high temperature to break the foaming body in the heating process to form more pore structures, keeping the temperature for 6 hours, and naturally cooling to room temperature to obtain the light honeycomb molecular sieve.
Further, the stirring time in the sample preliminary mixing step was 20 minutes, and the temperature was controlled to be 30 ℃.
Further, stirring and kneading in the sample pugging step
The temperature is controlled to be 35 ℃, and the stirring speed is 50 r/min.
Further, in the extrusion molding step, the temperature is controlled to be 30 ℃ during extrusion, the extrusion rate is 20mm/s, and the extrusion pressure is controlled
Further, in the low-temperature drying step, the temperature is controlled to be 30 +/-5 ℃, and the humidity is kept to be
The wind speed is lower than 2m/s, and the light is avoided; controlling the water loss rate of the wet blank to be 0.5%/d, ventilating once every 4 hours
Further, in the calcining step, the temperature rising rate is 3 ℃/min, the temperature is raised from the room temperature to 550 ℃ for calcining, and the temperature is kept at 550 ℃ for 6 h.
Further, the clay was 1250 mesh calcined kaolin.
Further, the foaming agent is one or more of sodium carboxymethylcellulose and soybean meal.
Further, the surfactant is composed of water, glycerol, polyethylene glycol and a silica sol solution, and the surfactant comprises the following components in percentage by mass: 70-80% of water, 10-15% of silica sol and 5-10% of glycerin and polyethylene glycol.
The invention has the beneficial effects that: according to the invention, by adding the organic binder and the foaming agent, on the basis of not influencing the mechanical strength of the whole structure of the honeycomb molecular sieve, more hollow structures are obtained by artificially controlling foaming and pore-forming, so that the whole density of the honeycomb molecular sieve is reduced, the specific surface area of a honeycomb molecular sieve module is increased, the contact adsorption of waste gas components and the honeycomb molecular sieve is facilitated, and the unit effective adsorption capacity is improved.
Drawings
FIG. 1 is a flow chart of a method of making a lightweight honeycomb molecular sieve purification module according to an embodiment of the present invention.
FIG. 2 is a schematic representation of the BET multipoint method specific surface area of a honeycomb molecular sieve in accordance with an embodiment of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application can be combined with each other without conflict, and the present invention is further described in detail with reference to the drawings and specific embodiments.
If directional indications (such as up, down, left, right, front, and rear … …) are provided in the embodiment of the present invention, the directional indications are only used to explain the relative position relationship between the components, the movement, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indications are changed accordingly.
In addition, the descriptions related to "first", "second", etc. in the present invention are only used for descriptive purposes and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature.
Referring to fig. 1, the preparation method of the lightweight honeycomb molecular sieve purification module according to the embodiment of the present invention includes a sample primary mixing step, a sample pugging step, an extrusion molding step, a low temperature drying step, a low temperature foaming step, and a calcining step.
A sample initial mixing step: weighing the following raw materials in percentage by weight: 60-80% of molecular sieve raw powder, 25-15% of binder, 10-3% of surfactant and 5-2% of foaming agent; and putting the weighed molecular sieve raw powder, the binder and the foaming agent into a mixer, and stirring and mixing the materials uniformly, wherein the binder is clay. The invention uses natural zeolite or artificially synthesized molecular sieve raw powder, and because the molecular sieve raw powder is powdery, the direct application is greatly limited, and particularly in the field of environmental protection, the powdery purifying material has large filling resistance and serious material loss, thereby greatly restricting the engineering application of the molecular sieve. According to the invention, more hollow structures are obtained by co-extruding and foaming the molecular sieve, the adhesive and the foaming agent, so that the overall density of the molecular sieve honeycomb module is reduced, the specific surface area of the molecular sieve module is increased, and the contact adsorption of waste gas components and the molecular sieve is facilitated.
A sample pugging step: adding the weighed surfactant, continuously stirring, putting the uniformly stirred mud-shaped blank into a mud mill, repeatedly mixing and extruding to obtain the well-mixed mud material, and controlling the temperature of the mud material to be
Coarse smelting is repeated for 5 times, and vacuum degree is
An extrusion molding step: and (3) putting the smelted pug into a low-pressure vacuum extruder for molding and extruding to obtain a wet blank.
And (3) low-temperature drying: and (3) placing the wet green body in a low-temperature drying environment, drying to remove excessive water, and reducing the water content of the wet green body to 18%.
And (3) low-temperature foaming step: and (3) foaming the wet blank at a low temperature of 80-90 ℃, keeping the temperature for 24h, and naturally cooling to room temperature to obtain a blank containing the naturally air-dried foam.
And (3) calcining: and (3) calcining the blank at high temperature to break the foaming body in the heating process to form more pore structures, keeping the temperature for 6 hours, and naturally cooling to room temperature to obtain the light honeycomb molecular sieve purification module.
The invention relates to a light honeycomb molecular sieve prepared by combining a foaming principle on the basis of honeycomb forming of the molecular sieve. Based on the influence of temperature and humidity on a molecular sieve material in an extrusion process, the problems of easiness in drying and cracking of a module, deformation of appearance, uneven wall thickness and the like in a preparation process exist. The invention mixes the molecular sieve, the adhesive, the foaming agent and the like for the first time, and obtains the honeycomb molecular sieve purification module with light weight, large specific surface and developed pore structure by optimizing the extrusion conditions and adopting the processes of low-pressure extrusion, low-temperature drying and high-temperature program calcination.
As an embodiment, the stirring time in the sample preliminary mixing step is 20 minutes, and the temperature is controlled to be 30 ℃.
As an embodiment, the sample is stirred and kneaded in the pugging step
The temperature is controlled to be 35 ℃, and the stirring speed is 50 r/min.
As an embodiment, in the extrusion molding step, the temperature is controlled to be 30 ℃ during extrusion, the extrusion rate is controlled to be 20mm/s, and the extrusion pressure is controlled to be
In one embodiment, the low-temperature drying step is performed at a temperature of 30 + -5 deg.C and a humidity of 30 + -5 deg.C
The wind speed is lower than 2m/s, and the light is avoided; controlling the water loss rate of the wet blank to be 0.5%/d, ventilating once every 4 hours
In one embodiment, in the calcination step, the temperature is raised from room temperature to 550 ℃ at a rate of 3 ℃/min, and the temperature is kept at 550 ℃ for 6 h.
As an embodiment, the clay is 1250 mesh calcined kaolin.
In one embodiment, the foaming agent is one or more of sodium carboxymethylcellulose and soybean meal.
As an implementation mode, the surfactant comprises water, glycerol, polyethylene glycol and a silica sol solution, and the surfactant comprises the following components in percentage by mass: 70-80% of water, 10-15% of silica sol and 5-10% of glycerin and polyethylene glycol. Water, glycerol, polyethylene glycol are surface active.
Firstly, mixing a plurality of binders, a molecular sieve and a foaming agent for pugging; and secondly, low-pressure extrusion molding is adopted, the mixture is placed for aging and then is dried at low temperature to remove excessive moisture, and finally, the mixture is calcined at high temperature through a program to obtain the lightweight honeycomb molecular sieve purification module with a strong framework structure, high mechanical strength, developed pore structure and large specific surface area.
Example 1:
(1) a sample initial mixing step: 40kg of molecular sieve raw material, 5.0kg of 1250-mesh calcined kaolin powder, 0.5kg of sodium carboxymethyl cellulose and 1.0kg of foaming agent are put into a mixer to be stirred and mixed uniformly for 20 minutes, and the temperature is controlled at 30 ℃.
(2) A sample pugging step: 30.0kg of water and 0.6kg of glycerin and polyethylene glycol, 0.2kg of a silica sol solution were added to the above (1) at a rate of 5 kg/min, and the mixture was further kneaded with stirring
Controlling the temperature at 35 ℃, stirringThe stirring speed is 50 r/min. The uniformly stirred mud-shaped blank is put into a mud mixer for repeated mixing and extrusion, and the temperature of the mud is controlled
Coarse smelting is repeated for 5 times, and vacuum degree is
(3) An extrusion molding step: and (3) putting the smelted pug into a low-pressure vacuum extruder for molding extrusion, wherein the extrusion temperature is controlled to be 30 ℃, the extrusion speed is 20mm/s, and the extrusion pressure is 30 MPa. (extrusion die external dimension: 100mm gamma 100mm square specification, pore structure hexagonal, aperture 3mm, wall thickness 1mm, green body cutting length 150 mm.)
(4) And (3) low-temperature drying: controlling the temperature to 30 +/-5 ℃ and maintaining the humidity
The wind speed is lower than 2m/s, the green body is protected from light, and the water loss rate of the wet green body is controlled to be 0.5%/d. Ventilating at intervals of 4 hours each time
The water content of the sample is reduced to 18%, and the sample is wetted to obtain a blank.
(5) And (3) low-temperature foaming step: and (3) foaming the wet blank at a low temperature of 80-90 ℃ for 24h, and naturally cooling to room temperature to obtain a naturally air-dried foam.
(6) And (3) calcining: and (3) calcining the blank in the step (5), heating the blank at a heating rate of 3 ℃/min, and carrying out programmed calcination at room temperature to 550 ℃, so that the foaming body is broken in the heating process to form more pore structures, keeping the temperature of 550 ℃ for 6h, and naturally cooling to room temperature to obtain the lightweight honeycomb molecular sieve purification module. The mechanical strength of the material is 1.77MPa, a sample is taken and 300mg is taken, the degassing temperature is 200 ℃, the degassing time is 300min, the ambient temperature is 20 ℃, and the specific surface area is tested to be 1322.1740m2The test is shown in figure 2 and tables 1, 2 and 3, wherein the compression strength (internal self-test) of the material is shown in table 1, and the specific surface test node of the BET multipoint method is shown in table 2Table 3 shows the results of the BJH pore size volume analysis.
TABLE 1
TABLE 2
TABLE 3
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A preparation method of a light honeycomb molecular sieve purification module is characterized by comprising the following steps:
a sample initial mixing step: weighing the following raw materials in percentage by weight: 60-80% of molecular sieve raw powder, 25-15% of binder, 10-3% of surfactant and 5-2% of foaming agent; putting the weighed molecular sieve raw powder, a binder and a foaming agent into a mixer, stirring and mixing the materials uniformly, wherein the binder is clay;
a sample pugging step: adding the weighed surfactant, continuously stirring, putting the uniformly stirred mud-shaped blank into a mud refining machine, repeatedly mixing and extruding to obtain refined mud, controlling the temperature of the mud to be 20-30 ℃, carrying out rough refining for 5 times, and vacuumizing to ensure that the vacuum degree is 10-15 KPa;
an extrusion molding step: putting the smelted pug into a low-pressure vacuum extruder for molding and extruding to obtain a wet blank;
and (3) low-temperature drying: placing the wet green body in a low-temperature drying environment, drying to remove excessive water, and reducing the water content of the wet green body to 18%;
and (3) low-temperature foaming step: foaming the wet blank at a low temperature of 80-90 ℃ for 24h, and naturally cooling to room temperature to obtain a blank containing a naturally air-dried foam;
and (3) calcining: and (3) calcining the blank at high temperature to break the foaming body in the heating process to form more pore structures, keeping the temperature for 6 hours, and naturally cooling to room temperature to obtain the light honeycomb molecular sieve.
2. The method of claim 1 wherein the sample is initially mixed for 20 minutes at a temperature of 30 ℃.
3. The preparation method of the light honeycomb molecular sieve purification module as claimed in claim 1, wherein in the sample pugging step, stirring and kneading are carried out for 20-30 min, the temperature is controlled to be 35 ℃, and the stirring speed is 50 r/min.
4. The preparation method of the light honeycomb molecular sieve purification module of claim 1, wherein in the extrusion molding step, the temperature is controlled to be 30 ℃ during extrusion, the extrusion rate is 20mm/s, and the extrusion pressure is 1-30 MPa.
5. The method of claim 1 wherein in the low temperature drying step, the temperature is controlled to 30 ± 5 ℃, the humidity is maintained at 75-85%, the wind speed is below 2m/s, and the light is shielded from light; controlling the water loss rate of the wet blank to be 0.5%/d, and ventilating once every 4 hours for 10-20 min.
6. The method for preparing the light weight honeycomb molecular sieve purification module of claim 1, wherein in the calcination step, the temperature rise rate is 3 ℃/min, the calcination is carried out from room temperature to 550 ℃, and the temperature is kept at 550 ℃ for 6 h.
7. The method of making a lightweight honeycomb molecular sieve purification module of claim 1, wherein the clay is 1250 mesh calcined kaolin.
8. The method of making a lightweight cellular molecular sieve purification module of claim 1, wherein the foaming agent is one or more of sodium carboxymethylcellulose, soy flour.
9. The method for preparing the light-weight cellular molecular sieve purification module according to claim 1, wherein the surfactant comprises water, glycerol, polyethylene glycol and a silica sol solution, and the surfactant comprises the following components in percentage by mass: 70-80% of water, 10-15% of silica sol and 5-10% of glycerin and polyethylene glycol.
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