CN111059894B - Continuous vacuum drying and roasting method for small-grain 5A molecular sieve - Google Patents
Continuous vacuum drying and roasting method for small-grain 5A molecular sieve Download PDFInfo
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- CN111059894B CN111059894B CN202010014725.1A CN202010014725A CN111059894B CN 111059894 B CN111059894 B CN 111059894B CN 202010014725 A CN202010014725 A CN 202010014725A CN 111059894 B CN111059894 B CN 111059894B
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
- F27B5/04—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated adapted for treating the charge in vacuum or special atmosphere
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- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
- F27B5/06—Details, accessories, or equipment peculiar to furnaces of these types
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
- F27B5/06—Details, accessories, or equipment peculiar to furnaces of these types
- F27B5/13—Arrangement of devices for discharging
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
- F27B5/06—Details, accessories, or equipment peculiar to furnaces of these types
- F27B5/18—Arrangement of controlling, monitoring, alarm or like devices
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28B—STEAM OR VAPOUR CONDENSERS
- F28B1/00—Condensers in which the steam or vapour is separate from the cooling medium by walls, e.g. surface condenser
- F28B1/02—Condensers in which the steam or vapour is separate from the cooling medium by walls, e.g. surface condenser using water or other liquid as the cooling medium
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28B—STEAM OR VAPOUR CONDENSERS
- F28B9/00—Auxiliary systems, arrangements, or devices
- F28B9/08—Auxiliary systems, arrangements, or devices for collecting and removing condensate
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Abstract
The invention relates to a continuous vacuum drying roasting method for a small-grain 5A molecular sieve, which comprises the following steps: filling a material 5A molecular sieve in a feeding tank; vacuumizing the feeding tank; vacuumizing the vertical disc rotary vacuum roasting furnace; sucking the 5A molecular sieve into a vertical disc rotary vacuum roasting furnace for sectional heating to obtain the dried, roasted and activated 5A molecular sieve; fourthly, vacuumizing a product bin; fifthly, opening the automatic control valve V of the feed inlet II of the product bin, and automatically closing the automatic control valve V after the weighing system of the product bin displays that the tank is full; sixthly, cooling to 50 ℃ in a product bin through a jacket to obtain a product; discharge of the products from the product silo; and meanwhile, the standby product bin is switched to be started. The invention has the advantages of accurate temperature control, safety and environmental protection, and can realize continuous operation under high vacuum degree.
Description
Technical Field
The invention relates to the technical field of novel drying, roasting and activating of materials sensitive to oxygen content and water vapor, in particular to a continuous vacuum drying and roasting method for a small-crystal-grain 5A molecular sieve.
Background
The special 5A molecular sieve adsorbent is prepared from a small-grain molecular sieve, and during roasting, the structure of the molecular sieve is greatly influenced by the moisture content in the roasting atmosphere, the moisture content is high, a hydrothermal environment is formed in a furnace body, the structure of the molecular sieve is damaged, and the performance of the adsorbent is further influenced. According to years of research, the adsorption capacity reduction range of the product can be reduced and the adsorption capacity of the product can be improved by adopting a vacuum oven drying roasting mode, but industrial application results show that the roasting mode has the problems that the temperature in the roasting atmosphere is not easy to control, the quality is low, scalding accidents are easy to occur in the production process and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a continuous vacuum drying and roasting method for a small-grain 5A molecular sieve, which can realize continuous operation, accurate temperature control and good safety.
In order to solve the problems, the invention provides a continuous vacuum drying roasting method for a small-grain 5A molecular sieve, which comprises the following steps:
the method comprises the steps of opening a self-control valve I on a feeding hole I of a feeding tank, closing a self-control valve II on a discharging hole I of the feeding tank, and starting to load the 5A molecular sieve until the loading is finished;
starting a vacuum pump II, and vacuumizing the feeding tank through an air exhaust port I to ensure that the vacuum degree is not less than-0.08 MPa (G);
thirdly, starting a vacuum pump I, and vacuumizing the vertical disc rotary vacuum roasting furnace to ensure that the vacuum degree is not less than-0.08 MPa (G); at the moment, opening a self-control valve II of a discharge port I of the feeding tank to enable the 5A molecular sieve to be sucked into the vertical disc rotary vacuum roasting furnace;
the 5A molecular sieve enters a first-stage temperature rising section, namely a first heating zone, when the temperature rises from 20 ℃ to 150 ℃, the 5A molecular sieve enters a first-stage constant temperature section, namely a second heating zone, from the first-stage temperature rising section, and the temperature is kept constant for 0.5 hour at 150 ℃; then, the 5A molecular sieve enters a second constant temperature raising section, namely a third heating zone, from the first constant temperature raising section, when the temperature is raised from 150 ℃ to 450 ℃, the 5A molecular sieve enters a second constant temperature raising section, namely a fourth heating zone, from the second temperature raising section, and the temperature is kept at 450 ℃ for 0.5 hour, so that the 5A molecular sieve and the non-condensable gas A after drying, roasting and activating are respectively obtained; the non-condensable gas A enters a condenser from a gas outlet at the top of the vertical disc rotary vacuum roasting furnace;
fourthly, closing an automatic control valve III of a discharge port II of a product bin, opening an automatic control valve IV of an air exhaust port II of the product bin, starting a vacuum pump II, and vacuumizing the product bin to ensure that the vacuum degree of the product bin is not less than-0.08 MPa (G);
fifthly, opening the automatic control valve V of the feed inlet II of the product bin, and automatically closing the automatic control valve V of the feed inlet II after a weighing system of the product bin displays that the tank is full;
sixthly, cooling to 50 ℃ in the product bin through a jacket to respectively obtain a product and a non-condensable gas B; the non-condensable gas B is sucked and discharged through the vacuum pump II;
opening a self-control valve VI connected with the atmosphere in an air suction port II, opening a self-control valve III of the discharge port II for discharging, and discharging the product from the discharge port II of the product bin; simultaneously switching and starting a standby product bin;
the non-condensable gas A and the non-condensable gas B are cooled by the condenser and then enter a collecting tank to respectively obtain a condensate and tail gas; the condensate is discharged through a condensed water discharge pipe at the bottom of the collection tank; and the tail gas is discharged from the top of the collecting tank through a vacuum pump I.
The shaft end seal of the vertical disc rotary vacuum roasting furnace is a structure of a filler and a sealing ring, and the axial seal adopts three-stage seal.
The top and the bottom of the vertical disc rotary vacuum roasting furnace are respectively provided with a cooling water inlet and outlet I and a cooling water inlet and outlet II, a total of 4 independent heating zones are arranged in the vertical disc rotary vacuum roasting furnace from top to bottom, and each heating zone is provided with N heating disc sheets according to heat load.
The product bin and the side of the standby product bin are both provided with jackets with cooling water inlets and cooling water outlets.
The condenser is in a shell-and-tube or fin type, and the side surface of the condenser is respectively provided with a cooling water upper water pipe and a cooling water return pipe.
And the vacuum pump I and the vacuum pump II are both water ring vacuum pumps.
Compared with the prior art, the invention has the following advantages:
1. high automation degree, accurate temperature control and good product quality.
The vertical disc rotary vacuum roasting furnace has high automation degree, the drying and roasting temperature is independently controlled and accurate, the temperature is controlled by the multilayer heating discs to form a heating gradient, the activation and roasting of the 5A molecular sieve are integrated, the adsorption strength and the adsorption capacity of the adsorbent are improved, and the product quality is superior to that of the original product.
2. The shaft end seal of the vertical disc rotary vacuum roasting furnace adopts a 'packing + sealing ring' structure, the axial seal adopts three-stage seal, the structure effectively prevents dust from being accumulated on a sealing contact surface, improves the service cycle of packing, effectively prevents high-temperature powder and high-temperature gas in a furnace cylinder from leaking, and has strong heat preservation and insulation performance and high heat efficiency; meanwhile, the filler is cooled by adopting cooling water around the filler, so that the problem of vacuum degree reduction caused by gaps due to fatigue caused by high-temperature expansion of the filler under the condition of long-time operation is solved.
3. Continuous operation, safety and environmental protection.
The invention adopts continuous operation, has small labor intensity and good sealing effect, can prevent dry materials from leaking, effectively avoids scalding accidents in the production process, and is safe and sanitary.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a schematic structural diagram of the present invention.
In the figure: 1-vertical disc rotary vacuum roasting furnace; 2-a feed tank; 31-a product bin; 32-a spare product bin; 4-a condenser; 5-a collection tank; 6-vacuum pump I; 7-vacuum pump II.
Detailed Description
As shown in fig. 1, a continuous vacuum drying and roasting method for a small-grain 5A molecular sieve comprises the following steps:
opening a self-control valve I on a feeding port I of a feeding tank 2, closing a self-control valve II on a discharging port I of the feeding tank 2, and starting to load a 5A molecular sieve until the loading is finished;
secondly, a vacuum pump II 7 is started, and the feeding tank 2 is vacuumized through the air extraction port I, so that the vacuum degree is not less than-0.08 MPa (G);
thirdly, starting a vacuum pump I6, and vacuumizing the vertical disc rotary vacuum roasting furnace 1 to ensure that the vacuum degree is not less than-0.08 MPa (G); at the moment, opening a self-control valve II of a discharge port I of the feeding tank 2 to enable the 5A molecular sieve to be sucked into the vertical disc rotary vacuum roasting furnace 1;
the 5A molecular sieve enters a first-stage temperature rising section, namely a first heating zone, when the temperature rises from 20 ℃ to 150 ℃, the 5A molecular sieve enters a first-stage constant temperature section, namely a second heating zone, from the first-stage temperature rising section, and the temperature is kept constant at 150 ℃ for 0.5 hour; then, the 5A molecular sieve enters a second constant temperature raising section, namely a third heating zone, from the first constant temperature raising section, when the temperature is raised from 150 ℃ to 450 ℃, the 5A molecular sieve enters a second constant temperature raising section, namely a fourth heating zone, from the second temperature raising section, and the temperature is kept at 450 ℃ for 0.5 hour, so that the 5A molecular sieve and the non-condensable gas A after drying, roasting and activating are respectively obtained; the non-condensable gas A enters a condenser 4 from a gas outlet at the top of the vertical disc rotary vacuum roasting furnace 1;
fourthly, closing an automatic control valve III of a discharge port II of the product bin 31, opening an automatic control valve IV of an air exhaust port II of the product bin 31, starting a vacuum pump II 7, and vacuumizing the product bin 31 to enable the vacuum degree to be not less than-0.08 MPa (G);
fifthly, opening the automatic control valve V of the feed inlet II of the product bin 31, and automatically closing the automatic control valve V of the feed inlet II after the weighing system of the product bin 31 displays that the tank is full;
sixthly, cooling to 50 ℃ in a product bin 31 through a jacket to obtain a product and a non-condensable gas B respectively; the non-condensable gas B is pumped and discharged by a vacuum pump II 7;
opening a self-control valve VI connected with the atmosphere in an air suction port II, opening a self-control valve III of a discharge port II for discharging, and discharging the product from a discharge port II of a product bin 31; while switching on the standby product bin 32; the two are used alternately to achieve the purpose of continuous operation.
The non-condensable gas A and the non-condensable gas B are cooled by a condenser 4 and then enter a collecting tank 5 to respectively obtain condensate and tail gas; the condensate is discharged through a condensed water discharge pipe at the bottom of the collection tank 5; the tail gas is discharged from the top of the collecting tank 5 through a vacuum pump I6.
Wherein: the shaft end seal of the vertical disc rotary vacuum roasting furnace 1 is a packing and sealing ring structure, and the axial seal adopts three-stage seal.
The top and the bottom of the vertical disc rotary vacuum roasting furnace 1 are respectively provided with a cooling water inlet and outlet I and a cooling water inlet and outlet II, 4 independent heating zones are arranged in the vertical disc rotary vacuum roasting furnace from top to bottom, and N heating disc sheets are arranged in each heating zone according to heat load.
The side surfaces of the product bin 31 and the standby product bin 32 are both provided with jackets with cooling water inlets and cooling water outlets.
The condenser 4 is in the form of a shell-and-tube or a fin type, and the side surface of the condenser is respectively provided with a cooling water upper water pipe and a cooling water return pipe.
And the vacuum pump I6 and the vacuum pump II 7 are water ring vacuum pumps.
Claims (6)
1. A continuous vacuum drying and roasting method for a small-grain 5A molecular sieve comprises the following steps:
the method comprises the steps of opening a self-control valve I on a feeding port I of a feeding tank (2), closing a self-control valve II on a discharging port I of the feeding tank (2), and starting to load the 5A molecular sieve until the loading is finished;
starting a vacuum pump II (7), and vacuumizing the feeding tank (2) through the air extraction port I to ensure that the vacuum degree is not less than-0.08 MPa (G);
thirdly, starting a vacuum pump I (6), and vacuumizing the vertical disc rotary vacuum roasting furnace (1) to ensure that the vacuum degree is not less than-0.08 MPa (G); at the moment, opening a self-control valve II of a discharge port I of the feeding tank (2) to enable the 5A molecular sieve to be sucked into the vertical disc rotary vacuum roasting furnace (1);
the 5A molecular sieve enters a first-stage temperature rising section, namely a first heating zone, when the temperature rises from 20 ℃ to 150 ℃, the 5A molecular sieve enters a first-stage constant temperature section, namely a second heating zone, from the first-stage temperature rising section, and the temperature is kept constant for 0.5 hour at 150 ℃; then, the 5A molecular sieve enters a second constant temperature raising section, namely a third heating zone, from the first constant temperature raising section, when the temperature is raised from 150 ℃ to 450 ℃, the 5A molecular sieve enters a second constant temperature raising section, namely a fourth heating zone, from the second temperature raising section, and the temperature is kept at 450 ℃ for 0.5 hour, so that the 5A molecular sieve and the non-condensable gas A after drying, roasting and activating are respectively obtained; the non-condensable gas A enters a condenser (4) from a gas outlet at the top of the vertical disc rotary vacuum roasting furnace (1);
fourthly, closing an automatic control valve III of a discharge port II of a product bin (31), opening an automatic control valve IV of an air suction port II of the product bin (31), starting a vacuum pump II (7), and vacuumizing the product bin (31) to ensure that the vacuum degree is not less than-0.08 MPa (G);
fifthly, opening the automatic control valve V of the feed inlet II of the product bin (31), and automatically closing the automatic control valve V of the feed inlet II after the weighing system of the product bin (31) displays full tank;
sixthly, cooling to 50 ℃ in the product bin (31) through a jacket to respectively obtain a product and noncondensable gas B; the non-condensable gas B is sucked and discharged through the vacuum pump II (7);
opening a self-control valve VI connected with the atmosphere in an air suction port II, opening a self-control valve III of the discharge port II for discharging, and discharging the product from the discharge port II of the product bin (31); simultaneously switching to start a standby product bin (32);
the non-condensable gas A and the non-condensable gas B are cooled by the condenser (4) and then enter a collecting tank (5) to respectively obtain a condensate and tail gas; the condensate is discharged through a condensed water discharge pipe at the bottom of the collection tank (5); and the tail gas is discharged from the top of the collecting tank (5) through a vacuum pump I (6).
2. The continuous vacuum drying roasting method for the small-grain 5A molecular sieve of claim 1, which is characterized by comprising the following steps of: the shaft end seal of the vertical disc rotary vacuum roasting furnace (1) is a filler + sealing ring structure, and the axial seal adopts three-stage seal.
3. The continuous vacuum drying roasting method for the small-grain 5A molecular sieve of claim 2, which is characterized by comprising the following steps of: the top and the bottom of the vertical disc rotary vacuum roasting furnace (1) are respectively provided with a cooling water inlet and outlet I and a cooling water inlet and outlet II, 4 independent heating zones are arranged from top to bottom in the vertical disc rotary vacuum roasting furnace, and each heating zone is provided with N heating disc sheets according to heat load.
4. The continuous vacuum drying roasting method for the small-grain 5A molecular sieve of claim 1, which is characterized by comprising the following steps of: the side surfaces of the product bin (31) and the standby product bin (32) are both provided with jackets with cooling water inlets and cooling water outlets.
5. The continuous vacuum drying roasting method for the small-grain 5A molecular sieve of claim 1, which is characterized by comprising the following steps of: the condenser (4) is in a shell-and-tube or fin type, and the side surface of the condenser is respectively provided with a cooling water upper water pipe and a cooling water return pipe.
6. The continuous vacuum drying roasting method for the small-grain 5A molecular sieve of claim 1, which is characterized by comprising the following steps of: the vacuum pump I (6) and the vacuum pump II (7) are both water-ring vacuum pumps.
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| CN113834293B (en) * | 2021-10-18 | 2023-03-24 | 中触媒新材料股份有限公司 | Device and method for water vapor desorption drying of low-silica-alumina-ratio molecular sieve |
| CN114377722B (en) * | 2021-12-29 | 2024-02-27 | 延长中科（大连）能源科技股份有限公司 | Regeneration method of molecular sieve catalyst |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN200982795Y (en) * | 2006-09-21 | 2007-11-28 | 国家粮食储备局郑州科学研究设计院 | Low temperature vacuum continuous drying tower for cereal |
| CN103090675A (en) * | 2011-11-02 | 2013-05-08 | 天华化工机械及自动化研究设计院有限公司 | Continuous vacuum drying and roasting combined method and device thereof |
| CN104841370A (en) * | 2015-04-09 | 2015-08-19 | 天华化工机械及自动化研究设计院有限公司 | Upright vacuum sealed type "drying-firing" method for PX spherical adsorbent |
| CN208154928U (en) * | 2018-05-11 | 2018-11-27 | 邹平双飞成套设备有限公司 | A kind of dry materials cooling tower |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN200982795Y (en) * | 2006-09-21 | 2007-11-28 | 国家粮食储备局郑州科学研究设计院 | Low temperature vacuum continuous drying tower for cereal |
| CN103090675A (en) * | 2011-11-02 | 2013-05-08 | 天华化工机械及自动化研究设计院有限公司 | Continuous vacuum drying and roasting combined method and device thereof |
| CN104841370A (en) * | 2015-04-09 | 2015-08-19 | 天华化工机械及自动化研究设计院有限公司 | Upright vacuum sealed type "drying-firing" method for PX spherical adsorbent |
| CN208154928U (en) * | 2018-05-11 | 2018-11-27 | 邹平双飞成套设备有限公司 | A kind of dry materials cooling tower |
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