CN111921564A - Reinforcing agent for reinforcing adhesion capability of catalyst-loaded silicon-aluminum-phosphorus molecular sieve and filling device suitable for catalyst - Google Patents
Reinforcing agent for reinforcing adhesion capability of catalyst-loaded silicon-aluminum-phosphorus molecular sieve and filling device suitable for catalyst Download PDFInfo
- Publication number
- CN111921564A CN111921564A CN202010817934.XA CN202010817934A CN111921564A CN 111921564 A CN111921564 A CN 111921564A CN 202010817934 A CN202010817934 A CN 202010817934A CN 111921564 A CN111921564 A CN 111921564A
- Authority
- CN
- China
- Prior art keywords
- catalyst
- furnace body
- aluminum
- molecular sieve
- ceramic honeycomb
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 96
- -1 silicon-aluminum-phosphorus Chemical compound 0.000 title claims abstract description 57
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 53
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000011049 filling Methods 0.000 title claims abstract description 41
- 239000012744 reinforcing agent Substances 0.000 title claims abstract description 36
- 230000003014 reinforcing effect Effects 0.000 title claims description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 78
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 64
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 34
- 239000000654 additive Substances 0.000 claims abstract description 27
- 230000000996 additive effect Effects 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 7
- 239000004375 Dextrin Substances 0.000 claims abstract description 7
- 229920001353 Dextrin Polymers 0.000 claims abstract description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 7
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 7
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 7
- 235000019425 dextrin Nutrition 0.000 claims abstract description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims abstract description 5
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims abstract description 4
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims abstract description 4
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011347 resin Substances 0.000 claims abstract description 4
- 229920005989 resin Polymers 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 244000275012 Sesbania cannabina Species 0.000 claims abstract 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract 2
- 239000000919 ceramic Substances 0.000 claims description 60
- 238000003756 stirring Methods 0.000 claims description 42
- 229910052751 metal Inorganic materials 0.000 claims description 37
- 239000002184 metal Substances 0.000 claims description 37
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 36
- 239000002002 slurry Substances 0.000 claims description 30
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- 239000011148 porous material Substances 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 22
- 239000000126 substance Substances 0.000 claims description 21
- 239000010963 304 stainless steel Substances 0.000 claims description 18
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- 238000005216 hydrothermal crystallization Methods 0.000 claims description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 12
- 239000012066 reaction slurry Substances 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- 239000004643 cyanate ester Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 239000003623 enhancer Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 230000001174 ascending effect Effects 0.000 claims 2
- 238000004804 winding Methods 0.000 claims 2
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 239000000853 adhesive Substances 0.000 abstract description 6
- 230000001070 adhesive effect Effects 0.000 abstract description 6
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 239000012948 isocyanate Substances 0.000 abstract 1
- 150000002513 isocyanates Chemical class 0.000 abstract 1
- 238000012856 packing Methods 0.000 description 21
- 238000001308 synthesis method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000005429 filling process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 241000219782 Sesbania Species 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 239000011949 solid catalyst Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910000954 Medium-carbon steel Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000005465 channeling Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012549 training Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/82—Phosphates
- B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
- B01J29/85—Silicoaluminophosphates [SAPO compounds]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
Abstract
The invention provides a reinforcing agent for enhancing the adhesion capability of a catalyst-loaded silicon-aluminum-phosphorus molecular sieve and a filling device suitable for the catalyst. The reinforcing agent mainly comprises a main agent, an auxiliary agent and an additive, wherein the main agent mainly comprises aluminum sol or silica sol, ammonia water, hydrochloric acid or nitric acid and desalted water; the auxiliary agent mainly comprises polyvinyl alcohol, carboxymethyl cellulose, dextrin or sesbania powder; the additive mainly comprises isocyanate, alkylphenol polyoxyethylene ether or dioctyl phthalate or vinyl acetate resin. The reinforcing agent can enhance the adhesive capacity of the silicon-aluminum-phosphorus molecular sieve on a cordierite carrier, so that more silicon-aluminum-phosphorus molecular sieves are adsorbed on the whole catalyst, and higher conversion rate and selectivity are achieved on a filled device. By using the filling device, the filling amount of the whole catalyst can be increased by 20-40%, so that the resistance of the whole catalyst in the furnace tube is basically consistent, and no blockage or bridging occurs.
Description
Technical Field
The invention relates to the field of chemical catalyst filling, in particular to a reinforcing agent for reinforcing the adhesion capability of a catalyst-loaded silicon-aluminum-phosphorus molecular sieve and a filling device suitable for the catalyst.
Background
With the upsizing of catalytic reactors and the development of technological levels, the filling technology and equipment of solid catalysts are becoming more and more important contents for the engineering development of catalysts. The method of charging the solid catalyst in the reactor is generally: the catalyst is loaded from the reactor inlet and allowed to fall freely. The catalyst has different packing densities due to different factors such as the falling speed, the packing time and the like of the catalyst, the falling speed is high, the packing time is long, the packing density of the catalyst is high, the falling speed is low, the packing time is short, and the packing density of the catalyst is low. Therefore, different packing causes different pressure drop of the catalyst bed, and the catalyst falls at a high speed and easily generates physical impact to break the catalyst or generate powder. Will certainly have certain influence on the experimental result.
The filling mode can be generally divided into normal filling and dense phase filling. The common filling is called sparse phase filling, cloth bag filling and dilute phase filling, and no external driving force is used in the filling process to improve the filling amount and the filling uniformity of the catalyst. The method is simple and easy to implement, special training is hardly required on personnel, and patent technology is not required on equipment, so that the method is adopted by many domestic enterprises. Dense phase packing can improve the handling capacity, has small airspeed, long device operation time, large packing bulk density, dense packing and large packing capacity, and can usually pack 10-25% more catalyst than the common packing method. Because the catalyst particles are regularly arranged on the cross section of the reactor during the filling process, the filling density of the catalyst particles along the longitudinal direction and the radial direction of the reactor is also very uniform. Dense phase packing has the following advantages: the reactor can be filled with more catalysts, so that the processing capacity is improved, the cycle is prolonged, and the product quality is improved; the dense-phase filling operation period is longer when the treatment capacity is the same; the catalyst bed layer is uniformly and closely filled, and can avoid the phenomena of bed layer collapse, channeling and the like, thereby avoiding the phenomenon of local overheating, the radial temperature of the catalyst layer is uniform, and the selectivity of the reaction can be improved. Dense phase packing is therefore more promising than normal packing.
If the catalyst is unevenly filled, the catalyst is easily to be short-circuited or the bed layer sinks, so that the distribution of materials and temperature in the reactor is uneven, the contact time of the materials and the catalyst is uneven, and the reaction pressure drop is uneven, thereby affecting the product quality and the service life of the catalyst. The core of the catalyst filling technology is to realize uniform filling of the catalyst in the filling process and improve the bulk density and the filling efficiency. At present, a plurality of companies at home and abroad develop a proprietary filling technology, and a favorable progress is made. However, many technical problems of catalyst loading remain to be solved.
The method of charging the solid catalyst in the fixed bed reactor is generally: the catalyst is loaded from the reactor inlet and allowed to fall freely. The catalyst has different packing densities due to different factors such as the falling speed, the packing time and the like of the catalyst, the falling speed is high, the packing time is long, the packing density of the catalyst is high, the falling speed is low, the packing time is short, and the packing density of the catalyst is low. Therefore, different pressure drops generated by different catalyst beds in different filling processes will certainly have certain influence on experimental results. Meanwhile, the catalyst falls at a high speed and physical impact is easily generated, so that the catalyst is broken or powder is generated.
Disclosure of Invention
In view of the above, the present invention is directed to a reinforcing agent for enhancing the adhesion of a catalyst-supported silicoaluminophosphate molecular sieve and a filling device suitable for the catalyst.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a reinforcing agent for reinforcing the adhesive ability of a catalyst-loaded silicon-aluminum-phosphorus molecular sieve comprises a main agent, an auxiliary agent and an additive, wherein the main agent comprises the following components in parts by mass: auxiliary agent: (ii) an additive (81-90): (8-18) 1, wherein the main agent comprises sol, ammonia water, acid and desalted water, and the preparation mass ratio is (70-84): (15-26): 1: (100- > 500); the auxiliary agent comprises polyvinyl alcohol, carboxymethyl cellulose and dextrin, and the preparation mass ratio of the auxiliary agent is (20-30): (40-50): (20-40); the additive mainly comprises cyanate ester and alkylphenol polyoxyethylene, and the preparation mass ratio of the cyanate ester to the alkylphenol polyoxyethylene is (90-95): (5-10).
Preferably, the sol is an aluminum sol or a silica sol, and the acid is hydrochloric acid or nitric acid.
Preferably, the dextrin is replaced by sesbania powder, and the alkylphenol polyoxyethylene is replaced by dioctyl phthalate or vinyl acetate resin.
The synthesis method of the enhancer comprises the following steps: step A1: selecting a 304 stainless steel reaction container A, adding a proper amount of desalted water, heating the reaction container A to 30-60 ℃, preserving heat, then adding the substances according to the sequence and proportion of the components of the main agent, stirring for 10-30min after each substance is added, and stirring all the substances after all the substances are added;
step A2: selecting a 304 stainless steel reaction container B, keeping the temperature at 20-40 ℃, and adding the auxiliary agent into the reaction container B to uniformly mix the components;
step A3: adding the uniformly stirred auxiliary agent in the reaction container B into the stirring reaction container A, and continuously stirring for 2-4 h;
step A4: selecting a 304 stainless steel reaction vessel C, keeping the temperature at 20-40 ℃, adding the components in the additive, stirring for 10-20min, adding the mixture into the reaction vessel A stirred in the step A3, keeping the temperature at 20-50 ℃, and continuously stirring the slurry in the reaction vessel A for 1-4h to prepare the reinforcing agent.
A method for preparing a catalyst loaded with a high-content silicon-aluminum-phosphorus molecular sieve by using the reinforcing agent comprises the following steps: step B1: selecting a cordierite ceramic honeycomb as a carrier, soaking the cordierite ceramic honeycomb in dilute nitric acid for 0.5 to 3 hours, taking out the cordierite ceramic honeycomb carrier, removing redundant dilute nitric acid in a pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting the cordierite ceramic honeycomb carrier;
step B2: putting the cordierite ceramic honeycomb carrier treated in the step B1 into the prepared reinforcing agent for soaking for 1-3h, then taking out, removing redundant slurry in the pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting;
step B3: and D, putting the cordierite ceramic honeycomb carrier treated in the step B2 into reaction slurry prepared from the silicon-aluminum-phosphorus molecular sieve for synthesis operation, wherein the silicon-aluminum-phosphorus molecular sieve generated in the reaction process is attached to the surface and in the pore channel of the cordierite ceramic honeycomb carrier, taking out the cordierite ceramic honeycomb carrier after the reaction is finished, removing redundant slurry in the pore channel, drying and roasting to obtain the monolithic catalyst loaded with the silicon-aluminum-phosphorus molecular sieve with higher content.
Further, the preparation method of the reaction slurry prepared from the silicoaluminophosphate molecular sieve in the step B3 comprises the following steps: stirring and mixing silica sol, pseudo-boehmite, phosphoric acid, triethylamine and desalted water at the temperature of 10-40 ℃ to prepare initial slurry of the silicon-aluminum-phosphorus molecular sieve, then carrying out hydrothermal crystallization on the slurry, wherein the temperature of the hydrothermal crystallization is 120 ℃ and 220 ℃, the time is 48-72h, and the proportion of the silica sol, the pseudo-boehmite, the phosphoric acid, the triethylamine and the desalted water is (0.1-2): 1: (0.5-2): (0.5-4): (100-200).
A filling device for a catalyst prepared by the method comprises a furnace body, a bottom support, a conveyor, a metal rope, a main wheel shaft and auxiliary wheel shafts, wherein the bottom support is placed in the furnace body in an inserting mode, a circle of upward slots are formed in the periphery of the bottom of the furnace body, the center of the bottom support protrudes downwards, a circle of downward slots are formed in the edge of the bottom support and are mutually inserted with the upward slots in the bottom of the furnace body, the main wheel shafts are arranged on the outer side above the furnace body, the number of the main wheel shafts is two and are vertically arranged, the number of the auxiliary wheel shafts is two, the auxiliary wheel shafts are hinged to a shaft rod, the shaft rod is hinged to the inner wall of the furnace body, the inner wall of the furnace body is provided with corresponding embedded grooves for placing the shaft rod and the auxiliary wheel shaft, the shaft rod is placed to be in a horizontal state due to the limit of the lower end face of the, the two auxiliary wheel shafts are respectively positioned on two opposite sides close to the bottom of the furnace body, the metal rope is sequentially wound on one main wheel shaft, the two auxiliary wheel shafts and the other main wheel shaft, a rope ring of the metal rope is gradually conveyed and wound on the other main wheel shaft from the one main wheel shaft, the conveyor is arranged on the edge of the upper end of the furnace body, and barbs at equal intervals are arranged on the metal rope.
The use method of the filling device comprises the following steps: step C1: cleaning the interior of the furnace body by using a wooden stick binding cloth, removing impurities in the furnace body, and then airing for 4-8 h to keep the interior of the furnace body in a thoroughly dried state;
step C2: the bottom support is placed at the bottom of the furnace body and is clamped on the slot at the bottom of the furnace body, so that the bottom support and the slot are ensured to be tightly contacted without leaving a gap;
step C3: initially, the metal ropes are wound on one main wheel shaft, and the other ends of the metal ropes are connected to the other main wheel shaft;
step C4: the catalyst is conveyed to the interior of the furnace body through the conveyor, the metal rope is gradually and completely wound on the other main wheel shaft from one main wheel shaft, and the barbs of the metal rope gradually eliminate gaps among the catalysts through the transmission of the metal rope, so that the catalyst is more compactly filled;
step C5: withdrawing the metal rope and the conveyor, and tightly connecting the upper end of the furnace body with the reaction system to finish the filling operation of the whole catalyst;
step C6: after the reaction, separating the reaction system, sleeving a collecting bag on the upper end of the furnace body, introducing compressed air upwards from the bottom outside the furnace body when discharging the catalyst in the furnace body, lifting the bottom support, and allowing the whole catalyst to enter the collecting bag along the upper end of the furnace body.
Furthermore, the linear speed of the rotation of the main wheel shaft is 0.3-0.6 times of the conveying speed of the conveyor.
Furthermore, the filling height of the whole catalyst is 80-95% of the height of the furnace body.
Compared with the prior art, the reinforcing agent for reinforcing the adhesion capability of the catalyst-loaded silicon-aluminum-phosphorus molecular sieve and the filling device suitable for the catalyst have the following advantages: the reinforcing agent can enable more silicon-aluminum-phosphorus molecular sieves to be attached to a cordierite carrier, the mass of the silicon-aluminum-phosphorus molecular sieves attached to the cordierite carrier using silica sol under the conventional condition is 15-21%, and after the reinforcing agent is used, the mass of the silicon-aluminum-phosphorus molecular sieves attached to the cordierite carrier can reach 20-30%, so that the catalytic performance of the whole catalyst on reaction is greatly improved, the conversion rate and the selectivity of the whole catalyst can be improved, and the service life of the whole catalyst can be prolonged.
By using the filling device to fill the monolithic catalyst, the filling amount of the monolithic catalyst can be increased by 20-40%, so that the resistance of the monolithic catalyst in the furnace tube is basically consistent, and no blockage or bridging occurs. After the filling device is used for filling, the reaction materials uniformly generate chemical reaction in the furnace tube, and the service life of the furnace tube can be prolonged. The device has high automation degree and is convenient for industrial popularization.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view of the construction of the filling device according to the present invention;
FIG. 2 is an enlarged view of portion A of FIG. 1;
description of reference numerals:
1-main wheel shaft; 2-furnace body; 3-auxiliary wheel shaft; 4-bottom support; 5-a metal cord; 6-barbs; 7-a conveyor; 8-embedding a groove; 9-shaft lever.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only 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," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; 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 meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
Example 1
A reinforcing agent for reinforcing the adhesive ability of a catalyst-loaded silicon-aluminum-phosphorus molecular sieve comprises a main agent, an auxiliary agent and an additive, wherein the main agent comprises the following components in parts by mass: auxiliary agent: additive 81: 8:1, wherein the main agent comprises alumina sol, ammonia water, hydrochloric acid and desalted water, and the preparation mass ratio is 70: 15: 1: 100, respectively; the auxiliary agent comprises polyvinyl alcohol, carboxymethyl cellulose and dextrin, and the preparation mass ratio is 20: 40: 20; the additive mainly comprises cyanate ester and alkylphenol polyoxyethylene, and the preparation mass ratio is 90: 5.
the synthesis method of the enhancer comprises the following steps: step A1: selecting a 304 stainless steel reaction container A, adding a proper amount of desalted water, heating the reaction container A to 30 ℃, preserving heat, then adding the substances according to the sequence and proportion of the components of the main agent, stirring for 10min after each substance is added, and stirring all the substances;
step A2: selecting a 304 stainless steel reaction container B, keeping the temperature at 20 ℃, and adding the components in the auxiliary agent to be uniformly mixed;
step A3: adding the uniformly stirred auxiliary agent in the reaction container B into the stirring reaction container A, and continuously stirring for 2 hours;
step A4: selecting a 304 stainless steel reaction vessel C, keeping the temperature at 20 ℃, adding the components in the additive, stirring for 10min, adding the mixture into the reaction vessel A stirred in the step A3, keeping the temperature at 20 ℃, and continuously stirring the slurry in the reaction vessel A for 1h to prepare the reinforcing agent.
A method for preparing a catalyst loaded with a high-content silicon-aluminum-phosphorus molecular sieve by using the reinforcing agent comprises the following steps: step B1: selecting a cordierite ceramic honeycomb as a carrier, soaking the cordierite ceramic honeycomb in dilute nitric acid for 0.5h, taking out the cordierite ceramic honeycomb carrier, removing redundant dilute nitric acid in a pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting the cordierite ceramic honeycomb carrier;
step B2: putting the cordierite ceramic honeycomb carrier treated in the step B1 into the prepared reinforcing agent for soaking for 1h, then taking out, removing redundant slurry in the pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting;
step B3: and D, putting the cordierite ceramic honeycomb carrier treated in the step B2 into reaction slurry prepared from the silicon-aluminum-phosphorus molecular sieve for synthesis operation, wherein the silicon-aluminum-phosphorus molecular sieve generated in the reaction process is attached to the surface and in the pore channel of the cordierite ceramic honeycomb carrier, taking out the cordierite ceramic honeycomb carrier after the reaction is finished, removing redundant slurry in the pore channel, drying and roasting to obtain the monolithic catalyst loaded with the silicon-aluminum-phosphorus molecular sieve with higher content.
The preparation method of the reaction slurry prepared from the silicon-aluminum-phosphorus molecular sieve in the step B3 comprises the following steps: stirring and mixing silica sol, pseudo-boehmite, phosphoric acid, triethylamine and desalted water at the temperature of 10-40 ℃ to prepare initial slurry of the silicon-aluminum-phosphorus molecular sieve, then carrying out hydrothermal crystallization on the slurry, wherein the hydrothermal crystallization temperature is 120 ℃, the hydrothermal crystallization time is 48h, and the ratio of the silica sol, the pseudo-boehmite, the phosphoric acid, the triethylamine and the desalted water is 0.1: 1: 0.5: 0.5: 100.
example 2
A reinforcing agent for reinforcing the adhesive ability of a catalyst-loaded silicon-aluminum-phosphorus molecular sieve comprises a main agent, an auxiliary agent and an additive, wherein the main agent comprises the following components in parts by mass: auxiliary agent: additive 90: 18:1, wherein the main agent comprises silica sol, ammonia water, nitric acid and desalted water, and the preparation mass ratio is 84: 26: 1: 500, a step of; the auxiliary agent comprises polyvinyl alcohol, carboxymethyl cellulose and sesbania powder, and the preparation mass ratio is 30: 50: 40; the additive mainly comprises cyanate ester and alkylphenol polyoxyethylene, and the preparation mass ratio is 95: 10.
the synthesis method of the enhancer comprises the following steps: step A1: selecting a 304 stainless steel reaction container A, adding a proper amount of desalted water, heating the reaction container A to 60 ℃, preserving heat, then adding the substances according to the sequence and proportion of the components of the main agent, stirring for 30min after each substance is added, and stirring all the substances;
step A2: selecting a 304 stainless steel reaction container B, keeping the temperature at 40 ℃, and adding the components in the auxiliary agent to be uniformly mixed;
step A3: adding the uniformly stirred auxiliary agent in the reaction container B into the stirring reaction container A, and continuously stirring for 4 hours;
step A4: selecting a 304 stainless steel reaction vessel C, keeping the temperature at 40 ℃, adding the components in the additive, stirring for 20min, adding the mixture into the reaction vessel A stirred in the step A3, keeping the temperature at 50 ℃, and continuously stirring the slurry in the reaction vessel A for 4h to prepare the reinforcing agent.
A method for preparing a catalyst loaded with a high-content silicon-aluminum-phosphorus molecular sieve by using the reinforcing agent comprises the following steps: step B1: selecting a cordierite ceramic honeycomb as a carrier, soaking the cordierite ceramic honeycomb in dilute nitric acid for 3 hours, taking out the cordierite ceramic honeycomb carrier, removing redundant dilute nitric acid in a pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting the cordierite ceramic honeycomb carrier;
step B2: putting the cordierite ceramic honeycomb carrier treated in the step B1 into the prepared reinforcing agent for soaking for 3 hours, then taking out, removing redundant slurry in the pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting;
step B3: and D, putting the cordierite ceramic honeycomb carrier treated in the step B2 into reaction slurry prepared from the silicon-aluminum-phosphorus molecular sieve for synthesis operation, wherein the silicon-aluminum-phosphorus molecular sieve generated in the reaction process is attached to the surface and in the pore channel of the cordierite ceramic honeycomb carrier, taking out the cordierite ceramic honeycomb carrier after the reaction is finished, removing redundant slurry in the pore channel, drying and roasting to obtain the monolithic catalyst loaded with the silicon-aluminum-phosphorus molecular sieve with higher content.
The preparation method of the reaction slurry prepared from the silicon-aluminum-phosphorus molecular sieve in the step B3 comprises the following steps: stirring and mixing silica sol, pseudo-boehmite, phosphoric acid, triethylamine and desalted water at 40 ℃ to prepare initial slurry of the silicon-aluminum-phosphorus molecular sieve, and then carrying out hydrothermal crystallization on the slurry, wherein the hydrothermal crystallization temperature is 220 ℃, the hydrothermal crystallization time is 72 hours, and the ratio of the silica sol, the pseudo-boehmite, the phosphoric acid, the triethylamine and the desalted water is 2: 1: 2: 4: 200.
example 3
A reinforcing agent for reinforcing the adhesive ability of a catalyst-loaded silicon-aluminum-phosphorus molecular sieve comprises a main agent, an auxiliary agent and an additive, wherein the main agent comprises the following components in parts by mass: auxiliary agent: additive 85: 12:1, wherein the main agent comprises alumina sol, ammonia water, nitric acid and desalted water, and the preparation mass ratio is 75: 20: 1: 200 of a carrier; the auxiliary agent comprises polyvinyl alcohol, carboxymethyl cellulose and dextrin, and the preparation mass ratio is 25: 45: 30, of a nitrogen-containing gas; the additive mainly comprises cyanate ester and dioctyl phthalate, and the preparation mass ratio is 92: 8.
the synthesis method of the enhancer comprises the following steps: step A1: selecting a 304 stainless steel reaction container A, adding a proper amount of desalted water, heating the reaction container A to 45 ℃, preserving heat, then adding the substances according to the sequence and proportion of the components of the main agent, stirring for 20min after each substance is added, and stirring all the substances;
step A2: selecting a 304 stainless steel reaction container B, keeping the temperature at 30 ℃, and adding the components in the auxiliary agent to be uniformly mixed;
step A3: adding the uniformly stirred auxiliary agent in the reaction container B into the stirring reaction container A, and continuously stirring for 3 hours;
step A4: selecting a 304 stainless steel reaction vessel C, keeping the temperature at 30 ℃, adding the components in the additive, stirring for 15min, adding the mixture into the reaction vessel A stirred in the step A3, keeping the temperature at 30 ℃, and continuously stirring the slurry in the reaction vessel A for 2h to prepare the reinforcing agent.
A method for preparing a catalyst loaded with a high-content silicon-aluminum-phosphorus molecular sieve by using the reinforcing agent comprises the following steps: step B1: selecting a cordierite ceramic honeycomb as a carrier, soaking the cordierite ceramic honeycomb in dilute nitric acid for 2 hours, taking out the cordierite ceramic honeycomb carrier, removing redundant dilute nitric acid in a pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting the cordierite ceramic honeycomb carrier;
step B2: putting the cordierite ceramic honeycomb carrier treated in the step B1 into the prepared reinforcing agent for soaking for 2 hours, then taking out, removing redundant slurry in the pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting;
step B3: and D, putting the cordierite ceramic honeycomb carrier treated in the step B2 into reaction slurry prepared from the silicon-aluminum-phosphorus molecular sieve for synthesis operation, wherein the silicon-aluminum-phosphorus molecular sieve generated in the reaction process is attached to the surface and in the pore channel of the cordierite ceramic honeycomb carrier, taking out the cordierite ceramic honeycomb carrier after the reaction is finished, removing redundant slurry in the pore channel, drying and roasting to obtain the monolithic catalyst loaded with the silicon-aluminum-phosphorus molecular sieve with higher content.
The preparation method of the reaction slurry prepared from the silicon-aluminum-phosphorus molecular sieve in the step B3 comprises the following steps: stirring and mixing silica sol, pseudo-boehmite, phosphoric acid, triethylamine and desalted water at the temperature of 20 ℃ to prepare initial slurry of the silicon-aluminum-phosphorus molecular sieve, and then carrying out hydrothermal crystallization on the slurry, wherein the hydrothermal crystallization temperature is 160 ℃, the hydrothermal crystallization time is 72 hours, and the ratio of the silica sol, the pseudo-boehmite, the phosphoric acid, the triethylamine and the desalted water is 1: 1: 1.5: 2: 150.
example 4
A reinforcing agent for reinforcing the adhesive ability of a catalyst-loaded silicon-aluminum-phosphorus molecular sieve comprises a main agent, an auxiliary agent and an additive, wherein the main agent comprises the following components in parts by mass: auxiliary agent: additive 90: 15:1, wherein the main agent comprises silica sol, ammonia water, hydrochloric acid and desalted water, and the preparation mass ratio is 84: 20: 1: 100, respectively; the auxiliary agent comprises polyvinyl alcohol, carboxymethyl cellulose and sesbania powder, and the preparation mass ratio is 25: 40: 35; the additive mainly comprises cyanate ester and vinyl acetate resin, and the preparation mass ratio is 90: 5.
the synthesis method of the enhancer comprises the following steps: step A1: selecting a 304 stainless steel reaction container A, adding a proper amount of desalted water, heating the reaction container A to 60 ℃, preserving heat, then adding the substances according to the sequence and proportion of the components of the main agent, stirring for 10min after each substance is added, and stirring all the substances;
step A2: selecting a 304 stainless steel reaction container B, keeping the temperature at 40 ℃, and adding the components in the auxiliary agent to be uniformly mixed;
step A3: adding the uniformly stirred auxiliary agent in the reaction container B into the stirring reaction container A, and continuously stirring for 2 hours;
step A4: selecting a 304 stainless steel reaction vessel C, keeping the temperature at 30 ℃, adding the components in the additive, stirring for 15min, adding the mixture into the reaction vessel A stirred in the step A3, keeping the temperature at 50 ℃, and continuously stirring the slurry in the reaction vessel A for 3h to prepare the reinforcing agent.
A method for preparing a catalyst loaded with a high-content silicon-aluminum-phosphorus molecular sieve by using the reinforcing agent comprises the following steps: step B1: selecting a cordierite ceramic honeycomb as a carrier, soaking the cordierite ceramic honeycomb in dilute nitric acid for 1h, taking out the cordierite ceramic honeycomb carrier, removing redundant dilute nitric acid in a pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting the cordierite ceramic honeycomb carrier;
step B2: putting the cordierite ceramic honeycomb carrier treated in the step B1 into the prepared reinforcing agent for soaking for 1h, then taking out, removing redundant slurry in the pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting;
step B3: and D, putting the cordierite ceramic honeycomb carrier treated in the step B2 into reaction slurry prepared from the silicon-aluminum-phosphorus molecular sieve for synthesis operation, wherein the silicon-aluminum-phosphorus molecular sieve generated in the reaction process is attached to the surface and in the pore channel of the cordierite ceramic honeycomb carrier, taking out the cordierite ceramic honeycomb carrier after the reaction is finished, removing redundant slurry in the pore channel, drying and roasting to obtain the monolithic catalyst loaded with the silicon-aluminum-phosphorus molecular sieve with higher content.
The preparation method of the reaction slurry prepared from the silicon-aluminum-phosphorus molecular sieve in the step B3 comprises the following steps: stirring and mixing silica sol, pseudo-boehmite, phosphoric acid, triethylamine and desalted water at 40 ℃ to prepare initial slurry of the silicon-aluminum-phosphorus molecular sieve, and then carrying out hydrothermal crystallization on the slurry, wherein the hydrothermal crystallization temperature is 220 ℃, the hydrothermal crystallization time is 72 hours, and the ratio of the silica sol, the pseudo-boehmite, the phosphoric acid, the triethylamine and the desalted water is 2: 1: 0.5: 0.5: 150.
example 5
As shown in the figure 1-2, the filling device for the catalyst prepared by the method comprises a furnace body 2, a bottom support 4, a conveyor 7, a metal rope 5, a main wheel shaft 1 and auxiliary wheel shafts 3, wherein the bottom support 4 is placed in the furnace body 2 in an insertion mode, a circle of upward slots are formed in the periphery of the bottom of the furnace body 2, the center of the bottom support 4 protrudes downwards, the edge of the bottom support 4 is a circle of downward slots which are mutually inserted with the upward slots in the bottom of the furnace body 2, the main wheel shaft 1 is arranged on the outer side above the furnace body 2, the main wheel shafts 1 are vertically arranged, the auxiliary wheel shafts 3 are provided with two auxiliary wheel shafts 3, the auxiliary wheel shafts 3 are hinged to a shaft lever 9, the shaft lever 9 is hinged to the inner wall of the furnace body 2, the inner wall of the furnace body 2 is provided with corresponding inner embedded grooves 8 for placing the shaft lever 9 and the auxiliary wheel shafts 3, and the shaft shafts 3 are, when the collet 4 is lifted up from bottom to top, the collet 4 drives the shaft lever 9 and the auxiliary wheel shaft 3 to upwards overturn to be embedded in the embedded groove 8, the two auxiliary wheel shafts 3 are respectively positioned at two opposite sides close to the bottom of the furnace body 2, the metal rope 5 sequentially winds one of the main wheel shaft 1, the two auxiliary wheel shafts 3 and the other main wheel shaft 1, the rope loop of the metal rope 5 is gradually conveyed and wound to the other main wheel shaft 1 from the main wheel shaft 1, the conveyor 7 is arranged at the edge of the upper end of the furnace body 2 and used for conveying a catalyst into the furnace body 2, and barbs 6 at equal intervals are arranged on the metal rope 5.
The use method of the filling device comprises the following steps: step C1: cleaning the interior of the furnace body 2 by using a wooden stick binding cloth, removing impurities in the furnace body 2, and then airing for 4-8 h to keep the interior of the furnace body 2 in a thoroughly dry state;
step C2: the bottom support 4 is placed at the bottom of the furnace body 2 and is clamped on the slot at the bottom of the furnace body 2, so that the bottom support and the slot are ensured to be tightly contacted without leaving a gap;
step C3: initially, the metal cords 5 are wound around one of the main wheel axles 1, so that the other ends of the metal cords 5 are connected to the other main wheel axle 1;
step C4: catalyst is conveyed to the interior of the furnace body 2 through a conveyor 7, the metal rope 5 is gradually and completely wound on the other main axle 1 from one main axle 1, and gaps among the catalyst are gradually eliminated through barbs 6 of the metal rope 5 through transmission of the metal rope 5, so that the catalyst is filled more compactly;
step C5: the metal rope 5 and the conveyor 7 are removed, the upper end of the furnace body 2 is tightly connected with the reaction system, and then the filling operation of the whole catalyst is completed;
step C6: after the reaction, the reaction system is separated, the upper end of the furnace body 2 is sleeved with a collecting bag, when the catalyst in the furnace body 2 is discharged, compressed air is upwards introduced from the bottom outside the furnace body 2, the bottom support 4 rises, and the whole catalyst enters the collecting bag along the upper end of the furnace body 2.
The metal rope 5 is an iron wire rope, and the length of the metal rope 5 is about 6.4-9.5 times of the height of the furnace body 2. The linear speed of the rotation of the main wheel shaft 1 is 0.3-0.6 times of the conveying speed of the conveyor 7. The filling height of the monolithic catalyst is 80-95% of the height of the furnace body 2.
The two main wheel shafts 1 run in opposite directions, i.e. when the lower main wheel shaft 1 runs counterclockwise, the upper main wheel shaft 1 runs clockwise. The metal rope 5 is distributed in the furnace body 2 in a ring shape, namely the metal rope 5 extends out from one main wheel shaft 1, then extends into the bottom of the furnace body 2 from one side of the furnace body 2, then turns over to extend out of the furnace body 2 upwards, and then is wound on the other main wheel shaft 1. The metal rope 5 is provided with a node at intervals of 10-20 cm. The node is provided with 6-10 barb 6 structures with the length of about 1-2 cm. The metal rope 5 is made of all-carbon material and has soft texture. The material of the barb 6 structure is high-quality 40# to 45# medium carbon steel, and the texture is very hard.
The diameter of the monolith catalyst to which the loading apparatus is applied is 1/10 or less in the diameter of the furnace tube.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A reinforcing agent for reinforcing the adhesion capability of a catalyst-loaded silicon-aluminum-phosphorus molecular sieve is characterized in that: the additive comprises a main agent, an auxiliary agent and an additive, and the main agent comprises the following components in parts by mass: auxiliary agent: (ii) an additive (81-90): (8-18) 1, wherein the main agent comprises sol, ammonia water, acid and desalted water, and the preparation mass ratio is (70-84): (15-26): 1: (100- > 500); the auxiliary agent comprises polyvinyl alcohol, carboxymethyl cellulose and dextrin, and the preparation mass ratio of the auxiliary agent is (20-30): (40-50): (20-40); the additive mainly comprises cyanate ester and alkylphenol polyoxyethylene, and the preparation mass ratio of the cyanate ester to the alkylphenol polyoxyethylene is (90-95): (5-10).
2. The reinforcing agent according to claim 1, characterized in that: the sol is aluminum sol or silica sol, and the acid is hydrochloric acid or nitric acid.
3. The reinforcing agent according to claim 1, characterized in that: the dextrin is replaced by sesbania powder, and the alkylphenol polyoxyethylene ether is replaced by dioctyl phthalate or vinyl acetate resin.
4. A method for synthesizing the enhancer of claim 1, wherein: the method comprises the following steps: step A1: selecting a 304 stainless steel reaction container A, adding a proper amount of desalted water, heating the reaction container A to 30-60 ℃, preserving heat, then adding the substances according to the sequence and proportion of the components of the main agent, stirring for 10-30min after each substance is added, and stirring all the substances after all the substances are added;
step A2: selecting a 304 stainless steel reaction container B, keeping the temperature at 20-40 ℃, and adding the auxiliary agent into the reaction container B to uniformly mix the components;
step A3: adding the uniformly stirred auxiliary agent in the reaction container B into the stirring reaction container A, and continuously stirring for 2-4 h;
step A4: selecting a 304 stainless steel reaction vessel C, keeping the temperature at 20-40 ℃, adding the components in the additive, stirring for 10-20min, adding the mixture into the reaction vessel A stirred in the step A3, keeping the temperature at 20-50 ℃, and continuously stirring the slurry in the reaction vessel A for 1-4h to prepare the reinforcing agent.
5. A method for preparing a catalyst loaded with a higher content of a silicoaluminophosphate molecular sieve by using the reinforcing agent of claim 1, wherein the method comprises the following steps: the method comprises the following steps: step B1: selecting a cordierite ceramic honeycomb as a carrier, soaking the cordierite ceramic honeycomb in dilute nitric acid for 0.5 to 3 hours, taking out the cordierite ceramic honeycomb carrier, removing redundant dilute nitric acid in a pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting the cordierite ceramic honeycomb carrier;
step B2: putting the cordierite ceramic honeycomb carrier treated in the step B1 into the prepared reinforcing agent for soaking for 1-3h, then taking out, removing redundant slurry in the pore channel of the cordierite ceramic honeycomb carrier, and then drying and roasting;
step B3: and D, putting the cordierite ceramic honeycomb carrier treated in the step B2 into reaction slurry prepared from the silicon-aluminum-phosphorus molecular sieve for synthesis operation, wherein the silicon-aluminum-phosphorus molecular sieve generated in the reaction process is attached to the surface and in the pore channel of the cordierite ceramic honeycomb carrier, taking out the cordierite ceramic honeycomb carrier after the reaction is finished, removing redundant slurry in the pore channel, drying and roasting to obtain the monolithic catalyst loaded with the silicon-aluminum-phosphorus molecular sieve with higher content.
6. The method of claim 5, wherein: the preparation method of the reaction slurry prepared from the silicon-aluminum-phosphorus molecular sieve in the step B3 comprises the following steps: stirring and mixing silica sol, pseudo-boehmite, phosphoric acid, triethylamine and desalted water at the temperature of 10-40 ℃ to prepare initial slurry of the silicon-aluminum-phosphorus molecular sieve, then carrying out hydrothermal crystallization on the slurry, wherein the temperature of the hydrothermal crystallization is 120 ℃ and 220 ℃, the time is 48-72h, and the proportion of the silica sol, the pseudo-boehmite, the phosphoric acid, the triethylamine and the desalted water is (0.1-2): 1: (0.5-2): (0.5-4): (100-200).
7. A loading device suitable for the catalyst prepared in claim 5 or 6, characterized in that: including furnace body (2), collet (4), conveyer (7), metal rope (5), main shaft (1) and auxiliary shaft (3), collet (4) are placed in furnace body (2) through the mode that can peg graft, be round ascending slot around furnace body (2) bottom, the center of collet (4) is protruding downwards, the edge of collet (4) is round decurrent slot, peg graft each other with furnace body (2) ascending slot in bottom, the outside of furnace body (2) top is located in main shaft (1), main shaft (1) is equipped with two, and vertical setting of arranging, auxiliary shaft (3) are equipped with two, auxiliary shaft (3) articulate in axostylus axostyle (9), axostylus axostyle (9) inner wall is equipped with corresponding interior caulking groove (8) that are used for axostylus axostyle (9) and auxiliary shaft (3) to place, auxiliary shaft (3) are because the spacing of interior caulking groove (8) lower terminal surface makes axostylus axostyle (9) put down in the natural state and are put down axostyl To the horizontality, when collet (4) lifted from bottom to top, collet (4) drive axostylus axostyle (9) and auxiliary shaft (3) upwards overturn to embedded in embedded groove (8), two auxiliary shaft (3) are located respectively and are close to furnace body (2) bottom relative both sides, one of them main shaft axle (1) of metal rope (5) winding in proper order, two auxiliary shaft (3) and another main shaft axle (1), the becket of metal rope (5) is carried gradually winding to another main shaft axle (1) from a main shaft axle (1), the edge of furnace body (2) upper end is located in conveyer (7), be equipped with equidistant spaced barb (6) on metal rope (5).
8. A method of using the filling device of claim 7, wherein: the method comprises the following steps: step C1: cleaning the interior of the furnace body (2) by using a wooden stick to bind the cloth, removing impurities in the furnace body (2), and then airing for 4-8 h to keep the interior of the furnace body (2) in a thoroughly dried state;
step C2: the bottom support (4) is placed at the bottom of the furnace body (2) and is clamped on a slot at the bottom of the furnace body (2), so that the bottom support and the slot are ensured to be tightly contacted without leaving a gap;
step C3: initially, the metal ropes (5) are wound on one main wheel shaft (1) so that the other ends of the metal ropes (5) are connected to the other main wheel shaft (1);
step C4: catalyst is conveyed to the interior of the furnace body (2) through a conveyor (7), the metal rope (5) is gradually and completely wound on the other main axle (1) from one main axle (1), and the barbs (6) of the metal rope (5) gradually eliminate gaps among the catalyst through transmission of the metal rope (5), so that the catalyst is filled more compactly;
step C5: the metal rope (5) and the conveyor (7) are removed, the upper end of the furnace body (2) is tightly connected with the reaction system, and then the filling operation of the whole catalyst is completed;
step C6: after the reaction, the reaction system is separated, the upper end of the furnace body (2) is sleeved with a collecting bag, when the catalyst in the furnace body (2) is discharged, compressed air is upwards introduced from the bottom outside the furnace body (2), the bottom support (4) rises, and the whole catalyst enters the collecting bag along the upper end of the furnace body (2).
9. Use according to claim 8, characterized in that: the linear speed of the rotation of the main wheel shaft (1) is 0.3-0.6 times of the conveying speed of the conveyor (7).
10. Use according to claim 8, characterized in that: the filling height of the whole catalyst is 80-95% of the height of the furnace body (2).
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010817934.XA CN111921564B (en) | 2020-08-14 | 2020-08-14 | Reinforcing agent for reinforcing adhesive capacity of catalyst-loaded silicon-aluminum-phosphorus molecular sieve and filling device suitable for catalyst |
| CN202310116768.4A CN115999450A (en) | 2020-08-14 | 2020-08-14 | Filling device of catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010817934.XA CN111921564B (en) | 2020-08-14 | 2020-08-14 | Reinforcing agent for reinforcing adhesive capacity of catalyst-loaded silicon-aluminum-phosphorus molecular sieve and filling device suitable for catalyst |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310116768.4A Division CN115999450A (en) | 2020-08-14 | 2020-08-14 | Filling device of catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111921564A true CN111921564A (en) | 2020-11-13 |
| CN111921564B CN111921564B (en) | 2023-04-21 |
Family
ID=73310933
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310116768.4A Pending CN115999450A (en) | 2020-08-14 | 2020-08-14 | Filling device of catalyst |
| CN202010817934.XA Active CN111921564B (en) | 2020-08-14 | 2020-08-14 | Reinforcing agent for reinforcing adhesive capacity of catalyst-loaded silicon-aluminum-phosphorus molecular sieve and filling device suitable for catalyst |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310116768.4A Pending CN115999450A (en) | 2020-08-14 | 2020-08-14 | Filling device of catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN115999450A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100304958A1 (en) * | 2006-10-16 | 2010-12-02 | Yun Guo | Method for preparing monolithic catalyst washcoat |
| CN104492473A (en) * | 2014-12-30 | 2015-04-08 | 华东理工大学 | Molecular sieve-coating cerium oxide composite material and preparation method thereof |
| CN106281050A (en) * | 2016-08-10 | 2017-01-04 | 无锡威孚环保催化剂有限公司 | A kind of preparation method and applications of molecular sieve SCR catalyst binding agent |
| CN107497473A (en) * | 2017-07-20 | 2017-12-22 | 沈阳化工大学 | A kind of Y molecular sieve method for preparing catalyst using cordierite as carrier |
| US20180022648A1 (en) * | 2015-12-25 | 2018-01-25 | Shandong Guiyuan Advanced Ceramics Co., Ltd | Method for preparing support of molecular sieve membrane |
| CN108545759A (en) * | 2018-04-18 | 2018-09-18 | 中国天辰工程有限公司 | A kind of preparation method and its evaluating apparatus of the sial phosphorus molecular sieve of modification |
| CN108816224A (en) * | 2018-06-26 | 2018-11-16 | 中国天辰工程有限公司 | A kind of catalyst and preparation method handling the exhaust gas in the roasting of sial phosphorus molecular sieve |
| CN110981458A (en) * | 2019-12-27 | 2020-04-10 | 中国天辰工程有限公司 | Device for containing silicon-aluminum-phosphorus molecular sieve and preparation method thereof |
-
2020
- 2020-08-14 CN CN202310116768.4A patent/CN115999450A/en active Pending
- 2020-08-14 CN CN202010817934.XA patent/CN111921564B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100304958A1 (en) * | 2006-10-16 | 2010-12-02 | Yun Guo | Method for preparing monolithic catalyst washcoat |
| CN104492473A (en) * | 2014-12-30 | 2015-04-08 | 华东理工大学 | Molecular sieve-coating cerium oxide composite material and preparation method thereof |
| US20180022648A1 (en) * | 2015-12-25 | 2018-01-25 | Shandong Guiyuan Advanced Ceramics Co., Ltd | Method for preparing support of molecular sieve membrane |
| CN106281050A (en) * | 2016-08-10 | 2017-01-04 | 无锡威孚环保催化剂有限公司 | A kind of preparation method and applications of molecular sieve SCR catalyst binding agent |
| CN107497473A (en) * | 2017-07-20 | 2017-12-22 | 沈阳化工大学 | A kind of Y molecular sieve method for preparing catalyst using cordierite as carrier |
| CN108545759A (en) * | 2018-04-18 | 2018-09-18 | 中国天辰工程有限公司 | A kind of preparation method and its evaluating apparatus of the sial phosphorus molecular sieve of modification |
| CN108816224A (en) * | 2018-06-26 | 2018-11-16 | 中国天辰工程有限公司 | A kind of catalyst and preparation method handling the exhaust gas in the roasting of sial phosphorus molecular sieve |
| CN110981458A (en) * | 2019-12-27 | 2020-04-10 | 中国天辰工程有限公司 | Device for containing silicon-aluminum-phosphorus molecular sieve and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115999450A (en) | 2023-04-25 |
| CN111921564B (en) | 2023-04-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI614214B (en) | Method and apparatus for preparing molecular sieves and catalysts for catalytic cracking | |
| CN111482203B (en) | Method for molding hollow spherical carrier | |
| CN111921564A (en) | Reinforcing agent for reinforcing adhesion capability of catalyst-loaded silicon-aluminum-phosphorus molecular sieve and filling device suitable for catalyst | |
| EP1943014A1 (en) | Catalyst loading apparatus | |
| CN102614866A (en) | Honeycomb SCR smoke denitration catalyst embryoid body and preparation method thereof | |
| CN1258567A (en) | Macroporous Alpha-alumina and its preparation and application | |
| CN103785438B (en) | A kind of equipment preparing catalytic cracking catalyst | |
| CN103787352A (en) | Method for preparing molecular sieve | |
| US7597529B2 (en) | Method for filling a vertical tube with catalyst particles | |
| JP2004136267A (en) | Method of manufacturing catalyst | |
| CN103785436B (en) | A kind of equipment preparing catalytic cracking catalyst | |
| CN105621358B (en) | A kind of methane reforming hydrogen production process | |
| CN110732297B (en) | System and method for loading particles into a microchannel reactor | |
| KR100585285B1 (en) | Production process for catalyst | |
| CN114471743B (en) | Advanced oxidation catalyst containing ferric phosphate and preparation method thereof | |
| US20180078924A1 (en) | Catalyst treatment device and method for manufacturing same | |
| CN113351232A (en) | Spherical nano catalyst for synthesizing isobutyraldehyde by methanol and ethanol one-step method and preparation method thereof | |
| CN112337428A (en) | Super-efficient drying molecular sieve and preparation method thereof | |
| JP2017080742A (en) | Preparation method of ring catalyst for preparing acrolein and acrylic acid, and preparation method of acrolein and acrylic acid using the catalyst | |
| TWI579047B (en) | Methods and apparatus for preparing molecular sieves and catalyst for catalytic cracking | |
| CN115382524B (en) | Porous alpha-alumina carrier for preparing silver catalyst for ethylene oxide production by ethylene oxidation, silver catalyst and application | |
| CN218222467U (en) | Device for washing and drying active carbon without damage | |
| CN114963787A (en) | Flash calciner predrying apparatus | |
| CN110131986A (en) | A kind of material frame, vertical drying device and furnace drying method for carrier drying | |
| CN115400783B (en) | Cordierite carrier coated molecular sieve catalyst and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |