CN112007686A - Catalyst preparation process for continuous production of alkylbenzene - Google Patents

Catalyst preparation process for continuous production of alkylbenzene Download PDF

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Publication number
CN112007686A
CN112007686A CN202010947315.2A CN202010947315A CN112007686A CN 112007686 A CN112007686 A CN 112007686A CN 202010947315 A CN202010947315 A CN 202010947315A CN 112007686 A CN112007686 A CN 112007686A
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grinding
box
zeolite
steps
microwave
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韩世龙
徐小亮
王宇
杨进
王堃
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JIANGSU FEIYA CHEMICAL INDUSTRY CO LTD
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JIANGSU FEIYA CHEMICAL INDUSTRY CO LTD
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00Catalysts comprising molecular sieves
    • B01J29/04Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • B01J20/18Synthetic zeolitic molecular sieves
    • B01J20/183Physical conditioning without chemical treatment, e.g. drying, granulating, coating, irradiation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • B01J20/18Synthetic zeolitic molecular sieves
    • B01J20/186Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0027Powdering
    • B01J37/0036Grinding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/06Washing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/344Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
    • B01J37/346Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2/00Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms
    • C07C2/54Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition of unsaturated hydrocarbons to saturated hydrocarbons or to hydrocarbons containing a six-membered aromatic ring with no unsaturation outside the aromatic ring
    • C07C2/64Addition to a carbon atom of a six-membered aromatic ring
    • C07C2/66Catalytic processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2229/00Aspects of molecular sieve catalysts not covered by B01J29/00
    • B01J2229/10After treatment, characterised by the effect to be obtained
    • B01J2229/18After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself

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Abstract

The invention discloses a catalyst preparation process for continuous production of alkylbenzene, belonging to the field of chemical production, and the catalyst preparation process for continuous production of alkylbenzene comprises the following steps: putting natural zeolite particles into a preparation device for grinding; carrying out microwave radiation reaction on the ground zeolite; then, carrying out modification reaction on the natural zeolite by using 0.6mol/L sodium chloride solution; and finally, the zeolite is cleaned and dried to prepare the modified zeolite, and the natural zeolite can be prepared into the modified zeolite by adopting a process combining microwave radiation and sodium chloride solution modification, so that the adsorption capacity of the zeolite is improved, the difficulty in preparing the modified zeolite is reduced, the investment cost is effectively reduced, the economic benefit of preparing the modified zeolite is improved, the modified zeolite can be effectively applied to the continuous production of alkylbenzene, the production efficiency of the alkylbenzene is improved, fluorine and chlorine in the alkylbenzene production process are absorbed, and the environmental protection property in the alkylbenzene production process is improved.

Description

Catalyst preparation process for continuous production of alkylbenzene
Technical Field
The invention relates to the field of chemical production, in particular to a catalyst preparation process for continuous production of alkylbenzene.
Background
The alkylbenzene is obtained by taking olefin as a raw material and carrying out alkylation reaction on the olefin and benzene through a catalyst. At present, enterprises use hydrofluoric acid as a catalyst during alkylbenzene production, the catalyst hydrofluoric acid needs to be put in a single kettle during alkylbenzene production, alkylbenzene products can be obtained through a series of operations such as filtering and separation, the number of operation units is large, the operation units are complex, the solid waste generation amount is large, and although the hydrofluoric acid has obvious advantages in efficiency and product quality compared with an aluminum catalyst, the problems of high equipment investment and maintenance cost caused by the corrosivity of the catalyst are solved. And in some enterprises, solid aluminum trichloride or aluminum trichloride ionic liquid is used as a catalyst for producing alkylbenzene, but the process has serious environmental protection problems and product quality problems, and large-area industrialization is difficult to realize.
The current new technology uses a non-corrosive solid catalyst (F-SiO2-Al2O3) to achieve the alkylation of benzene and normal olefins to produce linear alkylbenzenes. The reactor is a fixed bed reactor, the reactants maintain a liquid phase for operation, and the reaction conditions are mild. The use of non-corrosive solid catalyst greatly simplifies the design, operation, safety protection and other problems of alkylation devices, and no special metal materials, pumps, valves and the like are needed, so that the alkylation device has high activity and high selectivity.
Although the solid catalyst adopting the technology effectively solves the problem that the production of alkylbenzene is not environment-friendly, the catalyst needs to be continuously washed for 24 hours in the process for preparing the solid catalyst, the process for preparing the solid catalyst is difficult, the overshoot is complex, the investment cost is high, and the economic benefit is low.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a catalyst preparation process for continuous production of alkylbenzene, which can prepare natural zeolite into modified zeolite by adopting a process combining microwave radiation and sodium chloride solution modification, improve the adsorption capacity of the zeolite, effectively reduce the difficulty in preparing the modified zeolite, has simple and convenient preparation process, effectively reduces the investment cost, improves the economic benefit of preparing the modified zeolite, improves the stability of the modified zeolite, can be effectively applied to continuous production of alkylbenzene, improves the production efficiency of alkylbenzene, absorbs fluorine and chlorine in the alkylbenzene production process, ensures that the alkylbenzene production overshoot is free from fluorine and chlorine, improves the environmental protection of the production overshoot, reduces the requirements on the material of alkylbenzene production equipment, and reduces the difficulty in alkylbenzene production.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A catalyst preparation process for continuous production of alkylbenzene comprises the following steps:
s1, putting 100-150g of natural zeolite particles into a preparation device for grinding;
s2, performing microwave radiation reaction on the ground natural zeolite in a preparation device;
s3, carrying out modification reaction on the zeolite subjected to microwave radiation reaction in a preparation device, and carrying out modification reaction on the zeolite by using 0.6mol/L sodium chloride solution, wherein the volume ratio of the 0.6mol/L sodium chloride solution to the natural zeolite is 3: 1-5: 1;
and S4, finally, cleaning and drying the modified zeolite in a preparation device to prepare the modified zeolite. The modified zeolite is prepared from natural zeolite by adopting a process combining microwave radiation and sodium chloride solution modification, so that the adsorption capacity of the zeolite is improved, the difficulty in preparing the modified zeolite is effectively reduced, the preparation process is simple and convenient, the investment cost is effectively reduced, the economic benefit for preparing the modified zeolite is improved, the stability of the modified zeolite is improved, the modified zeolite can be effectively applied to the continuous production of alkylbenzene, the production efficiency of the alkylbenzene is improved, fluorine and chlorine in the alkylbenzene production process are absorbed, the alkylbenzene production overshoot is free from fluorine and chlorine, the environmental protection of the alkylbenzene production overshoot is improved, the material requirement of alkylbenzene production equipment is reduced, and the difficulty in producing the alkylbenzene is reduced.
Further, the S2 and S3 steps are replaced with S2a and S3a steps, respectively:
s2a, carrying out modification reaction on the ground natural zeolite in a preparation device, and carrying out modification reaction on the natural zeolite by using 0.6mol/L sodium chloride solution;
and S3a, carrying out microwave radiation reaction on the modified zeolite in a preparation device.
Further, the intensity of the microwave radiation in the step S2 is 450-.
Further, in the step S3, the modification reaction temperature of the 0.6mol/L sodium chloride solution and the natural zeolite is 30-60 ℃, and the modification reaction time is 8-12 h.
Further, the preparation device comprises a machine body, wherein a grinding box, a microwave box, a modification box, a cleaning box and a drying box are fixedly installed in the machine body from top to bottom in sequence, the grinding box, the microwave box, the modification box, the cleaning box and the drying box are communicated in sequence, a grinding assembly is connected in the grinding box, a blanking assembly is connected in the microwave box, and valves are arranged on pipelines communicated among the modification box, the cleaning box and the drying box;
the grinding assembly comprises a grinding motor, the upper end of the machine body is fixedly provided with the grinding motor, the lower end of the grinding motor is fixedly connected with a grinding rotating rod, the lower end of the grinding rotating rod penetrates through the machine body and extends into the grinding box, the outer end of the grinding rotating rod is fixedly connected with an upper grinding block and a lower grinding block respectively, and the upper grinding block is located at the upper end of the lower grinding block. Modified zeolite is prepared by using a preparation device, and natural zeolite particles are ground by using a grinding assembly, so that the volume of the natural zeolite particles is reduced, the contact area of the natural zeolite particles during subsequent reaction is effectively increased, the reaction efficiency is effectively increased, and the modification quality is improved.
Furthermore, a plurality of material passing holes are formed in the lower grinding block, and a plurality of grinding lugs are fixedly connected to the lower end of the lower grinding block.
Furthermore, the grinding box is fixedly connected with a fixed block on the upper inner wall, the fixed block is rotatably connected with the grinding rotating rod, the fixed block is matched with the upper grinding block, the upper end of the grinding box is fixedly connected with a pair of feed hoppers communicated with the grinding box, the two feed hoppers are respectively positioned on the left side and the right side of the grinding motor, the upper end of each feed hopper extends out of the machine body, and the lower end of each feed hopper penetrates through the fixed block. Decide the piece and cooperate with grinding motor, carry out primary to natural zeolite and grind, the rethread is ground the piece down and is carried out the secondary and grind, effectively improves the grinding efficiency, improves the degree of consistency of grinding.
Further, the equal fixedly connected with deflector of inner wall about grinding case, and the deflector is located and grinds between piece and the lower grinding piece, inner wall fixedly connected with sieve under the grinding case, and sieve and lower grinding piece phase-match. The deflector leads the natural zeolite of whereabouts, screens the natural zeolite after grinding through the sieve, and effective control grinding precision effectively guarantees the efficiency of follow-up reaction.
Furthermore, microwave transmitting plates are fixedly mounted on the left inner wall and the right inner wall of the microwave box, and oscillators are fixedly mounted on the left inner wall and the right inner wall of the modification box.
Further, the unloading subassembly is including the unloading motor, organism rear end fixed mounting has the unloading motor, unloading motor output fixedly connected with unloading pivot, unloading pivot front end runs through the organism to extend to the microwave incasement, unloading pivot outer end fixedly connected with nested piece, the equal fixedly connected with striker plate in both ends about the nested piece, striker plate and microwave case phase-match. The striker plate shields natural zeolite entering the microwave box, after the striker plate is subjected to microwave radiation for enough time, the blanking motor drives the blanking rotating shaft to rotate, the striker plate is driven to turn over in the microwave box through the sleeve block, so that the natural zeolite falls, and meanwhile, the subsequent natural zeolite entering the microwave box is shielded, and the effectiveness of the microwave radiation is effectively ensured.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) according to the scheme, the technical process of combining microwave radiation and sodium chloride solution modification is adopted, natural zeolite is made into modified zeolite, the adsorption capacity of zeolite is improved, the difficulty of preparing modified zeolite is effectively reduced, the preparation process is simple and convenient, the investment cost is effectively reduced, the economic benefit of preparing modified zeolite is improved, the stability of modified zeolite is improved, the modified zeolite can be effectively applied to continuous production of alkylbenzene, the production efficiency of alkylbenzene is improved, fluorine and chlorine in the alkylbenzene production process are absorbed, the alkylbenzene production overshoot is free of fluorine and chlorine, the environment friendliness of production overshoot is improved, the material requirement of alkylbenzene production equipment is reduced, and the difficulty of alkylbenzene production is reduced.
(2) The S2a and S3a steps are used for replacing the S2 and S3 steps, so that the applicability of the preparation process of the catalyst can be effectively improved, the preparation device is effectively simplified, and the economic benefit of preparation is improved.
(3) By controlling the intensity and time of microwave radiation, the radiation efficiency of the natural zeolite is effectively improved, the radiation effect is improved, and the existing resources are reasonably utilized.
(4) By increasing the reaction temperature of the 0.6mol/L sodium chloride solution and the natural zeolite, the reaction efficiency is effectively improved, the reaction effect is enhanced, and the effectiveness of modification of the natural zeolite is effectively ensured.
(5) Modified zeolite is prepared by using a preparation device, and natural zeolite particles are ground by using a grinding assembly, so that the volume of the natural zeolite particles is reduced, the contact area of the natural zeolite particles during subsequent reaction is effectively increased, the reaction efficiency is effectively increased, and the modification quality is improved.
(6) Through the natural zeolite after the grinding of the upper grinding block, the material passing hole on the lower grinding block can effectively fall to the lower side inside the grinding box, and the shielding of the lower grinding block on the natural zeolite is effectively avoided.
(7) Decide the piece and cooperate with grinding motor, carry out primary to natural zeolite and grind, the rethread is ground the piece down and is carried out the secondary and grind, effectively improves the grinding efficiency, improves the degree of consistency of grinding.
(8) The deflector leads the natural zeolite of whereabouts, screens the natural zeolite after grinding through the sieve, and effective control grinding precision effectively guarantees the efficiency of follow-up reaction.
(9) The striker plate shields natural zeolite entering the microwave box, after the striker plate is subjected to microwave radiation for enough time, the blanking motor drives the blanking rotating shaft to rotate, the striker plate is driven to turn over in the microwave box through the sleeve block, so that the natural zeolite falls, and meanwhile, the subsequent natural zeolite entering the microwave box is shielded, and the effectiveness of the microwave radiation is effectively ensured.
Drawings
FIG. 1 is a schematic diagram of the process flow of the present invention using steps S2 and S3;
FIG. 2 is a schematic diagram of the process flow structure of the present invention using the steps S2a and S3 a;
FIG. 3 is a schematic cross-sectional view of the main body of the present invention;
FIG. 4 is a schematic cross-sectional front view of the grinding box of the present invention;
FIG. 5 is a schematic cross-sectional front view of an abrasive assembly of the present invention;
FIG. 6 is a schematic sectional view of the microwave box according to the present invention;
FIG. 7 is a schematic axial view of the blanking assembly of the present invention;
fig. 8 is a schematic structural diagram of a front view cross section of the modified box of the present invention.
The reference numbers in the figures illustrate:
1 machine body, 2 grinding boxes, 201 fixed blocks, 202 feed hoppers, 203 guide plates, 204 sieve plates, 3 microwave boxes, 301 microwave emission plates, 4 modification boxes, 401 oscillators, 5 cleaning boxes, 6 drying boxes, 7 grinding assemblies, 701 grinding motors, 702 grinding rotating rods, 703 upper grinding blocks, 704 lower grinding blocks, 705 material passing holes, 8 blanking assemblies, 801 blanking motors, 802 blanking rotating shafts, 803 sleeve blocks and 804 material baffle plates.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
referring to fig. 1, a catalyst preparation process for continuous production of alkylbenzene includes the following steps:
s1, putting 100-150g of natural zeolite particles into a preparation device for grinding;
s2, performing microwave radiation reaction on the ground natural zeolite in a preparation device;
s3, carrying out modification reaction on the zeolite subjected to microwave radiation reaction in a preparation device, and carrying out modification reaction on the zeolite by using 0.6mol/L sodium chloride solution, wherein the volume ratio of the 0.6mol/L sodium chloride solution to the natural zeolite is 3: 1-5: 1;
and S4, finally, cleaning and drying the modified zeolite in a preparation device to prepare the modified zeolite. The modified zeolite is prepared from natural zeolite by adopting a process combining microwave radiation and sodium chloride solution modification, so that the adsorption capacity of the zeolite is improved, the difficulty in preparing the modified zeolite is effectively reduced, the preparation process is simple and convenient, the investment cost is effectively reduced, the economic benefit for preparing the modified zeolite is improved, the stability of the modified zeolite is improved, the modified zeolite can be effectively applied to the continuous production of alkylbenzene, the production efficiency of the alkylbenzene is improved, fluorine and chlorine in the alkylbenzene production process are absorbed, the alkylbenzene production overshoot is free from fluorine and chlorine, the environmental protection of the alkylbenzene production overshoot is improved, the material requirement of alkylbenzene production equipment is reduced, and the difficulty in producing the alkylbenzene is reduced.
Referring to fig. 3-8, the preparation device comprises a machine body 1, wherein a grinding box 2, a microwave box 3, a modification box 4, a cleaning box 5 and a drying box 6 are fixedly arranged in the machine body 1 from top to bottom in sequence, the grinding box 2, the microwave box 3, the modification box 4, the cleaning box 5 and the drying box 6 are communicated in sequence, a grinding assembly 7 is connected in the grinding box 2, a blanking assembly 8 is connected in the microwave box 3, and a valve is arranged on a pipeline communicated among the modification box 4, the cleaning box 5 and the drying box 6; the grinding assembly 7 includes a grinding motor 701, the grinding motor 701 is prior art, and a person skilled in the art can select a suitable type of grinding motor 701 according to actual needs, for example: the grinding motor 701 of model Y90S-2, organism 1 upper end fixed mounting have grinding motor 701, grinding motor 701 lower extreme fixedly connected with grinds bull stick 702, grinds bull stick 702 lower extreme and runs through organism 1 to extend to grinding box 2 in, grinds bull stick 702 outer end fixedly connected with respectively and grinds piece 703 with grinding piece 704 down, and goes up grinding piece 703 and is located grinding piece 704 upper end down. Modified zeolite is prepared by using a preparation device, and natural zeolite particles are ground by using a grinding component 7, so that the volume of the natural zeolite particles is reduced, the contact area of the natural zeolite particles during subsequent reaction is effectively increased, the reaction efficiency is effectively increased, and the modification quality is improved.
Referring to fig. 4 and 5, the grinding box 2 has a fixed block 201 fixedly connected to the upper inner wall thereof, the fixed block 201 is rotatably connected to the grinding rotating rod 702, the fixed block 201 is matched with the upper grinding block 703, the upper end of the grinding box 2 is fixedly connected to a pair of feed hoppers 202 communicated therewith, the two feed hoppers 202 are respectively located at the left and right sides of the grinding motor 701, the upper end of the feed hopper 202 extends out of the machine body 1, and the lower end of the feed hopper 202 penetrates through the fixed block 201. Decide piece 201 and grinding motor 701 and cooperate, carry out primary grinding to natural zeolite, the rethread is ground piece 704 down and is carried out the secondary and grind, effectively improves the grinding efficiency, improves the degree of consistency of grinding.
Referring to fig. 4 and 5, the left and right inner walls of the grinding box 2 are both fixedly connected with the guide plate 203, the guide plate 203 is located between the upper grinding block 703 and the lower grinding block 704, the lower inner wall of the grinding box 2 is fixedly connected with the screen plate 204, and the screen plate 204 is matched with the lower grinding block 704. The guide plate 203 guides the falling natural zeolite, the ground natural zeolite is screened through the sieve plate 204, the grinding precision is effectively controlled, and the efficiency of subsequent reaction is effectively ensured.
Referring to fig. 3-8, microwave emitting plates 301 are fixedly mounted on left and right inner walls of the microwave box 3, the microwave emitting plates 301 are of the prior art and are not described in detail in the description, oscillators 401 are fixedly mounted on left and right inner walls of the modification box 4, the oscillators 401 are of the prior art and are not described in the description. The blanking assembly 8 comprises a blanking motor 801, the blanking motor 801 is the prior art, and a person skilled in the art can select a suitable type of blanking motor 801 according to actual needs, for example: the model is Y80M1-2 blanking motor 801, the blanking motor 801 is fixedly installed at the rear end of the machine body 1, the output end of the blanking motor 801 is fixedly connected with a blanking rotating shaft 802, the front end of the blanking rotating shaft 802 penetrates through the machine body 1 and extends into the microwave box 3, the outer end of the blanking rotating shaft 802 is fixedly connected with a sleeve block 803, the left end and the right end of the sleeve block 803 are fixedly connected with material blocking plates 804, and the material blocking plates 804 are matched with the microwave box 3. The baffle 804 shields the natural zeolite entering the microwave box 3, so that after the natural zeolite is irradiated by microwave for a sufficient time, the blanking motor 801 drives the blanking rotating shaft 802 to rotate, the baffle 804 is driven by the sleeve 803 to turn over in the microwave box 3, the natural zeolite falls, and meanwhile, the natural zeolite subsequently entering the microwave box 3 is shielded, thereby effectively ensuring the effectiveness of microwave radiation.
The using method comprises the following steps: particles of natural zeolite are fed into a grinding box 2 from a feed hopper 202, a grinding motor 701 is started, an upper grinding block 703 and a lower grinding block 704 are driven to rotate through a grinding rotating rod 702, the upper grinding block 703 is matched with a top block 201 to carry out primary grinding, and the lower grinding block 704 is matched with a sieve plate 204 to carry out secondary grinding; the qualified ground natural zeolite enters the microwave box 3 through the sieve plate, is shielded in the microwave box 3 through the material baffle 804, is subjected to microwave radiation through the microwave transmitting plate 301, and after the microwave radiation is finished, the blanking motor 801 is started, and the sleeve block 803 is driven to rotate 180 degrees through the blanking rotating shaft 802, so that the material baffle 804 is turned over 180 degrees; the zeolite after microwave radiation falls into the modification box 4 to react with the solution in the modification box 4, the oscillator 401 is started to improve the reaction efficiency, the zeolite is precipitated at the lower end of the modification box 4 after reaction and is discharged into the cleaning box 5 to be cleaned, the modified zeolite is dried by the drying box 6, and the modified zeolite is discharged.
Example 2:
referring to fig. 2, wherein the same or corresponding components as those in embodiment 1 are designated by the same reference numerals as those in embodiment 1, only the points different from embodiment 1 will be described below for the sake of convenience. This example 2 differs from example 1 in that: the S2 and S3 steps are replaced with S2a and S3a steps, respectively:
s2a, carrying out modification reaction on the ground natural zeolite in a preparation device, and carrying out modification reaction on the natural zeolite by using 0.6mol/L sodium chloride solution;
and S3a, carrying out microwave radiation reaction on the modified zeolite in a preparation device. The S2a and S3a steps are used for replacing the S2 and S3 steps, so that the applicability of the preparation process of the catalyst can be effectively improved, the preparation device is effectively simplified, and the economic benefit of preparation is improved.
Example 3:
referring to fig. 1, wherein the same or corresponding components as those in embodiment 1 are designated by the same reference numerals as those in embodiment 1, only the points different from embodiment 1 will be described below for the sake of convenience. This example 3 differs from example 1 in that: the intensity of the microwave radiation in step S2 is 450-470W, and the time of the microwave radiation is 8-12 min. By controlling the intensity and time of microwave radiation, the radiation efficiency of the natural zeolite is effectively improved, the radiation effect is improved, and the existing resources are reasonably utilized.
Example 4:
referring to fig. 1, wherein the same or corresponding components as those in embodiment 1 are designated by the same reference numerals as those in embodiment 1, only the points different from embodiment 1 will be described below for the sake of convenience. This example 4 differs from example 1 in that: in the step S3, the modification reaction temperature of the 0.6mol/L sodium chloride solution and the natural zeolite is 30-60 ℃, and the modification reaction time is 8-12 h. By increasing the reaction temperature of the 0.6mol/L sodium chloride solution and the natural zeolite, the reaction efficiency is effectively improved, the reaction effect is enhanced, and the effectiveness of modification of the natural zeolite is effectively ensured.
Example 5:
referring to fig. 3 to 6, wherein the same or corresponding components as those in embodiment 1 are designated by the same reference numerals as those in embodiment 1, only the points different from embodiment 1 will be described below for the sake of convenience. This example 5 differs from example 1 in that: a plurality of material passing holes 705 are formed in the lower grinding block 704, and a plurality of grinding lugs are fixedly connected to the lower end of the lower grinding block 704. The natural zeolite ground by the upper grinding block 703 can effectively fall to the lower side inside the grinding box 2 through the material passing hole 705 on the lower grinding block 704, and the shielding of the lower grinding block 704 on the natural zeolite is effectively avoided.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.

Claims (10)

1. A catalyst preparation process for continuous production of alkylbenzene is characterized by comprising the following steps: the method comprises the following steps:
s1, putting 100-150g of natural zeolite particles into a preparation device for grinding;
s2, performing microwave radiation reaction on the ground natural zeolite in a preparation device;
s3, carrying out modification reaction on the zeolite subjected to microwave radiation reaction in a preparation device, and carrying out modification reaction on the zeolite by using 0.6mol/L sodium chloride solution, wherein the volume ratio of the 0.6mol/L sodium chloride solution to the natural zeolite is 3: 1-5: 1;
and S4, finally, cleaning and drying the modified zeolite in a preparation device to prepare the modified zeolite.
2. The process of claim 1, wherein the catalyst is prepared by a method comprising the steps of: the S2 and S3 steps are replaced with S2a and S3a steps, respectively:
s2a, carrying out modification reaction on the ground natural zeolite in a preparation device, and carrying out modification reaction on the natural zeolite by using 0.6mol/L sodium chloride solution;
and S3a, carrying out microwave radiation reaction on the modified zeolite in a preparation device.
3. The process of claim 1, wherein the catalyst is prepared by a method comprising the steps of: the intensity of the microwave radiation in the step S2 is 450-470W, and the time of the microwave radiation is 8-12 min.
4. The process of claim 1, wherein the catalyst is prepared by a method comprising the steps of: in the step S3, the modification reaction temperature of the 0.6mol/L sodium chloride solution and the zeolite is 30-60 ℃, and the modification reaction time is 8-12 h.
5. The process of claim 1, wherein the catalyst is prepared by a method comprising the steps of: the preparation device comprises a machine body (1), wherein a grinding box (2), a microwave box (3), a modification box (4), a cleaning box (5) and a drying box (6) are fixedly installed in the machine body (1) from top to bottom in sequence, the grinding box (2), the microwave box (3), the modification box (4), the cleaning box (5) and the drying box (6) are communicated in sequence, a grinding assembly (7) is connected in the grinding box (2), a blanking assembly (8) is connected in the microwave box (3), and valves are arranged on pipelines communicated among the modification box (4), the cleaning box (5) and the drying box (6);
the grinding assembly (7) comprises a grinding motor (701), the upper end of the machine body (1) is fixedly provided with the grinding motor (701), the lower end of the grinding motor (701) is fixedly connected with a grinding rotating rod (702), the lower end of the grinding rotating rod (702) penetrates through the machine body (1) and extends into the grinding box (2), the outer end of the grinding rotating rod (702) is respectively and fixedly connected with an upper grinding block (703) and a lower grinding block (704), and the upper grinding block (703) is positioned at the upper end of the lower grinding block (704).
6. The process of claim 5, wherein the catalyst is prepared by a method comprising the steps of: a plurality of material passing holes (705) are formed in the lower grinding block (704), and a plurality of grinding convex blocks are fixedly connected to the lower end of the lower grinding block (704).
7. The process of claim 5, wherein the catalyst is prepared by a method comprising the steps of: the grinding machine is characterized in that a fixed block (201) is fixedly connected to the upper inner wall of the grinding box (2), the fixed block (201) is rotatably connected with a grinding rotating rod (702), the fixed block (201) is matched with an upper grinding block (703), a pair of feed hoppers (202) communicated with the grinding box (2) are fixedly connected to the upper end of the grinding box (2), the two feed hoppers (202) are respectively located on the left side and the right side of a grinding motor (701), a machine body (1) extends out of the upper end of each feed hopper (202), and the lower ends of the feed hoppers (202) penetrate through the fixed block (201).
8. The process of claim 5, wherein the catalyst is prepared by a method comprising the steps of: the grinding box is characterized in that the left inner wall and the right inner wall of the grinding box (2) are fixedly connected with guide plates (203), the guide plates (203) are located between an upper grinding block (703) and a lower grinding block (704), the lower inner wall of the grinding box (2) is fixedly connected with a sieve plate (204), and the sieve plate (204) is matched with the lower grinding block (704).
9. The process of claim 5, wherein the catalyst is prepared by a method comprising the steps of: microwave emission board (301) are all fixedly mounted on the left inner wall and the right inner wall of microwave box (3), and oscillator (401) are all fixedly mounted on the left inner wall and the right inner wall of modification box (4).
10. The process of claim 5, wherein the catalyst is prepared by a method comprising the steps of: unloading subassembly (8) is including unloading motor (801), organism (1) rear end fixed mounting has unloading motor (801), unloading motor (801) output end fixedly connected with unloading pivot (802), unloading pivot (802) front end runs through organism (1) to extend to in microwave case (3), unloading pivot (802) outer end fixedly connected with cover block (803), equal fixedly connected with striker plate (804) in both ends about cover block (803), striker plate (804) and microwave case (3) phase-match.
CN202010947315.2A 2020-09-10 2020-09-10 Catalyst preparation process for continuous production of alkylbenzene Pending CN112007686A (en)

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