CN112619273A - Device and method for recovering solvent from magnesium slag in Grignard section - Google Patents
Device and method for recovering solvent from magnesium slag in Grignard section Download PDFInfo
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- CN112619273A CN112619273A CN202011508921.0A CN202011508921A CN112619273A CN 112619273 A CN112619273 A CN 112619273A CN 202011508921 A CN202011508921 A CN 202011508921A CN 112619273 A CN112619273 A CN 112619273A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/14—Production of inert gas mixtures; Use of inert gases in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/26—Magnesium halides
- C01F5/30—Chlorides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
- C07D309/34—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D309/36—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with oxygen atoms directly attached to ring carbon atoms
- C07D309/40—Oxygen atoms attached in positions 3 and 4, e.g. maltol
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B23/00—Heating arrangements
- F26B23/10—Heating arrangements using tubes or passages containing heated fluids, e.g. acting as radiative elements; Closed-loop systems
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/001—Handling, e.g. loading or unloading arrangements
- F26B25/002—Handling, e.g. loading or unloading arrangements for bulk goods
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/009—Alarm systems; Safety sytems, e.g. preventing fire and explosions
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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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Abstract
The invention relates to a device and a method for recovering a solvent from magnesium slag in a Grignard working section, which are characterized in that: (1) putting the materials in the hydrolysis kettle into a double-cone vacuum drier; (2) temporarily connecting a discharge port valve at the end of a double-cone vacuum dryer welded with a perforated plate with an intermediate tank by using a pipeline, vacuumizing the liquid material to the intermediate tank, introducing nitrogen for protection, and removing the pipeline after the material pumping is finished; (3) controlling the pressure of a double-cone vacuum dryer to be below-0.086 MPa and the temperature to be 60-70 ℃; simultaneously controlling the temperature of a circulating water condenser and a frozen brine condenser, and keeping the liquid temperature at the outlet of the frozen brine condenser at 0-10 ℃; (4) and opening a discharge port valve at the end of the double-cone unwelded hole plate after no obvious distillation, and pouring out the basic magnesium chloride filter residue. The invention has the advantages that: the device has low investment cost and easy operation, and greatly reduces the manpower; the recovery efficiency is improved, and more nearly 300L of solvent can be recovered per day; the potential safety hazard in the transfer process is thoroughly solved, and the safety of the device is improved.
Description
Technical Field
The invention belongs to the technical field of chemical production, relates to production of maltol, and particularly relates to a device and a method for recovering a solvent from magnesium slag in a Grignard working section.
Background
The production process of maltol is divided into a Grignard working section, a chlorination working section, a sublimation working section, a crystallization working section and a drying working section; after the hydrolysis reaction in the Grignard section, the mixture (basic magnesium chloride, furfuryl alcohol, toluene and tetrahydrofuran solvent) after the reaction is put into a filter cylinder with filter cloth, the filtered filtrate is pumped into an intermediate tank by vacuum and collected, the filtered basic magnesium chloride filter residue is transported to a magnesium residue recovery position by a forklift, and then is poured into a rake dryer for drying, and the toluene and tetrahydrofuran solvent contained in the filter residue are recovered.
The method is complex to operate and low in recovery efficiency, the used rake dryer uses a 45Kwh motor, the occupied area is large, the energy consumption is high, toluene is 3.2 class-type flash-point flammable liquid, tetrahydrofuran is 3.1 class-type low-flash-point flammable liquid, and great potential safety hazards are easily caused when a forklift transports and puts materials into the rake dryer.
Disclosure of Invention
The invention aims to solve the problems and provides a device and a method for recovering a solvent from magnesium slag in a Grignard section.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a device for recovering solvent from magnesium slag in a Grignard section is characterized by comprising the following devices: the Grignard hydrolysis kettle is sequentially connected with a double-cone vacuum dryer, a vacuum pump, a circulating water condenser, a frozen brine condenser and a solvent recovery tank, wherein a control valve is welded at a discharge port at one end of the double-cone vacuum dryer, an orifice plate is welded inside the discharge port, the orifice plate is circular, small holes are uniformly distributed in the orifice plate, and filter cloth is arranged on the orifice plate.
Further, the pore plate is arranged at a position 20cm away from the discharge hole of the double-cone vacuum dryer.
Further, the control valve is a valve of DN 50.
Further, the diameter of the hole on the orifice plate is 2 mm.
Furthermore, the control valve is connected with a material pumping pipeline (which is installed as required).
A method for recovering a solvent from magnesium slag in a Grignard working section is characterized by comprising the following steps:
(1) putting the materials (the magnesium slag and the intermediate mixed liquid) in the hydrolysis kettle into a double-cone vacuum drier;
(2) temporarily connecting a discharge port valve (a valve of DN 50) at the end of a perforated plate welded on a bipyramid vacuum dryer with an intermediate tank by using a movable pipeline, pumping a liquid material (intermediate solution) in the bipyramid to an intermediate receiving tank by using vacuum (-0.05-0.095 MPa), introducing nitrogen gas for protection on a vacuum pumping pipeline, and detaching the pipeline connected with the bipyramid after the pumping is finished (no obvious liquid flow is observed from a material pumping pipeline sight glass);
(3) opening a vacuum valve on a double-cone vacuum dryer, controlling the pressure to be below-0.086 MPa, introducing hot water at the temperature of 55-80 ℃ into a jacket of the double-cone vacuum dryer, slowly heating, and controlling the temperature in the double-cone vacuum dryer to be 60-70 ℃; meanwhile, the temperature of a circulating water condenser and a frozen brine condenser is controlled, the temperature of liquid at the outlet of the frozen brine condenser is kept between 0 and 10 ℃ (in the later stage of distillation, the distillation yield is reduced obviously, and the temperature of hot water is properly increased);
(4) and after no obvious distillation exists, opening a discharge port valve at the end of the double-cone unwelded hole plate after drying, pouring out the dried basic magnesium chloride filter residue in the dryer by using a transfer tank, conveying the filter residue to a magnesium residue recovery station for next recovery, and pumping the recovered toluene and tetrahydrofuran solvent to a Grignard section for recycling.
Further, the temperature of the circulating water condenser is controlled to be 20-30 ℃, and the temperature of the frozen brine condenser is controlled to be-5 ℃.
In the Grignard hydrolysis discharge stage, explosive mixed gas is formed due to the fact that volatile gas containing toluene and tetrahydrofuran contacts with air, a small amount of nitrogen is introduced for protection for safety production, meanwhile, a discharge port valve at one end of a double-cone welded pore plate is connected with a pre-connected temporary vacuum material pumping pipeline, and an intermediate filtered by double-cone inner filter cloth is pumped into an intermediate receiving groove (solid-liquid filtration separation is carried out in the double cones); and in the drying stage, carrying out reduced pressure distillation on the filtered basic magnesium chloride, opening a double-cone discharge port after the distillation is finished, leading out the dried basic magnesium chloride by using a container, conveying the dried basic magnesium chloride to a magnesium slag recovery post for next recovery, and pumping the recovered toluene and tetrahydrofuran solvents to a Grignard section for recycling.
The invention has the advantages that: the device has low investment cost and easy operation, and can greatly reduce the manpower; compared with the drying mode of the prior rake dryer, the recovery efficiency is increased, and more nearly 300L of solvent can be recovered every day; the potential safety hazard in the transfer process is thoroughly solved, and the safety of the device is improved.
Drawings
FIG. 1 is a schematic view of a process for recovering a solvent from magnesium slag in a Grignard section;
fig. 2 is a schematic structural view of a double-cone vacuum dryer.
Detailed Description
The invention is further illustrated with reference to fig. 1 and 2:
a device for recovering solvent from magnesium slag in a Grignard section comprises the following equipment: a discharge valve at the bottom of the Grignard hydrolysis kettle is connected with a valve at the feeding port of the double-cone vacuum drier through a movable pipeline, a discharge valve at the end of the double-cone vacuum drier welded with a perforated plate (a valve of DN 50) is connected (temporarily connected) with a movable pipeline of the intermediate tank, and a discharge valve at the end of the double-cone vacuum drier not welded with the perforated plate is connected with a transfer tank; the double-cone vacuum drier is also sequentially connected with a vacuum pump, a circulating water condenser, a frozen brine condenser and a solvent recovery tank; the pore plate in the double-cone vacuum dryer is welded at a position 20cm away from the discharge port, the pore plate is circular, small holes (the diameter is 2 mm) are uniformly distributed in the pore plate, and filter cloth is arranged on the pore plate.
A method for recovering a solvent from magnesium slag in a Grignard section in maltol production comprises the following specific implementation steps:
example 1
(1) Opening a discharging valve at the bottom of the hydrolysis kettle, and putting 5000L of materials (magnesium slag and intermediate mixed liquid) in the hydrolysis kettle into a double-cone vacuum drier;
(2) temporarily connecting a discharge port valve (a valve of DN 50) at the end of a perforated plate welded by a double-cone vacuum dryer with an intermediate tank by using a movable pipeline, pumping a liquid material (Grignard intermediate solution) in the double cones to the intermediate receiving tank by using vacuum (-0.08 MPa), introducing nitrogen for protection on a vacuum pumping pipeline, finishing pumping after 30min (no obvious liquid flows out when observed from a viewing mirror of the pumping pipeline), detaching the pipeline connected with the double cones, and closing a pumping valve and a feeding port to obtain 3200L of liquid in the intermediate receiving tank;
(3) starting a vacuum pump, opening a vacuum valve on a double-cone vacuum dryer, starting a hot water valve at an inlet and an outlet of a double-cone jacket, controlling the pressure to be-0.08 MPa, introducing 65 ℃ hot water into the double-cone vacuum dryer jacket, slowly heating, and controlling the temperature in the double-cone vacuum dryer to be 60 ℃; simultaneously controlling the temperature of a circulating water condenser at 25 ℃, the temperature of a frozen brine condenser at 0 ℃, and enabling liquid (5 ℃) discharged from the frozen brine condenser to enter a solvent recovery tank;
(4) and (3) after 120min, opening a discharge port valve at the end of the double-cone unwelded hole plate, pouring out the dried basic magnesium chloride filter residue in the dryer by using a transfer tank, conveying the filter residue to a magnesium residue recovery station for next recovery, and pumping the recovered toluene and tetrahydrofuran solvent to a Grignard working section for recycling, wherein 300L of the liquid in the recovered solvent receiving tank is obtained.
Example 2
(1) Opening a discharging valve at the bottom of the hydrolysis kettle, and putting 5200L of materials (magnesium slag and intermediate mixed liquid) in the hydrolysis kettle into a double-cone vacuum drier;
(2) temporarily connecting a discharge port valve (a valve of DN 50) at the end of a perforated plate welded on a bipyramid vacuum dryer with an intermediate tank by using a movable pipeline, pumping a bipyramid internal liquid material (Grignard intermediate solution) to the intermediate receiving tank by using vacuum (-0.09 MPa), introducing nitrogen for protection on a vacuum pumping pipeline, finishing pumping after 35min (obviously no liquid flows out from a viewing mirror of the pumping pipeline), removing the pipeline connected with the bipyramid, and closing a pumping valve and a feeding port to obtain 3300L of intermediate receiving tank internal liquid;
(3) starting a vacuum pump, opening a vacuum valve on a double-cone vacuum dryer, starting a hot water valve at an inlet and an outlet of a double-cone jacket, controlling the pressure to be-0.05 MPa, introducing 80 ℃ hot water into the double-cone vacuum dryer jacket, slowly heating, and controlling the temperature in the double-cone vacuum dryer to be 75 ℃; simultaneously controlling the temperature of a circulating water condenser at 25 ℃, the temperature of a frozen brine condenser at 2 ℃, and enabling liquid (7 ℃) discharged from the frozen brine condenser to enter a solvent recovery tank;
(4) and after the drying is finished after 140min, opening a discharge port valve at the end of the double-cone unwelded hole plate, pouring out the dried basic magnesium chloride filter residue in the dryer by using a transfer tank, conveying the filter residue to a magnesium residue recovery station for next recovery, and pumping the recovered toluene and tetrahydrofuran solvent to a Grignard section for recycling, wherein 320L of the liquid in the recovered solvent receiving tank is obtained.
Example 3
(1) Opening a discharging valve at the bottom of the hydrolysis kettle, and putting 5000L of materials (magnesium slag and intermediate mixed liquid) in the hydrolysis kettle into a double-cone vacuum drier;
(2) temporarily connecting a discharge port valve (a valve of DN 50) at the end of a perforated plate welded on a bipyramid vacuum dryer with an intermediate tank by using a movable pipeline, pumping a bipyramid internal liquid material (Grignard intermediate solution) to the intermediate receiving tank by using vacuum (-0.07 MPa), introducing nitrogen for protection on a vacuum pumping pipeline, finishing pumping after 35min (no obvious liquid flows out when observed from a viewing mirror of the pumping pipeline), removing the pipeline connected with the bipyramid, and closing a pumping valve and a feeding port to obtain 3000L of intermediate receiving tank internal liquid;
(3) starting a vacuum pump, opening a vacuum valve on a double-cone vacuum dryer, starting a hot water valve at an inlet and an outlet of a double-cone jacket, controlling the pressure to be-0.07 MPa, introducing 75 ℃ hot water into the jacket of the double-cone vacuum dryer, slowly heating, and controlling the temperature in the double-cone vacuum dryer to be 70 ℃; simultaneously controlling the temperature of a circulating water condenser at 28 ℃, the temperature of a frozen brine condenser at 5 ℃, and enabling liquid (8 ℃) discharged from the frozen brine condenser to enter a solvent recovery tank;
(4) and after 110min, opening a discharge port valve at the end of the double-cone unwelded hole plate, pouring out the dried basic magnesium chloride filter residue in the dryer by using a transfer tank, conveying the filter residue to a magnesium residue recovery station for next recovery, and pumping the recovered toluene and tetrahydrofuran solvent to a Grignard working section for recycling, wherein 295L of liquid in the recovered solvent receiving tank is obtained.
By adopting the method, the recovered solvent is 300L more per kettle than the original method, the solvent is not in contact with the external environment in the whole operation process, and the peculiar smell of solvent volatilization is avoided during later-stage discharging, so that the potential safety hazard and the potential environmental hazard are eliminated.
Claims (7)
1. A device for recovering solvent from magnesium slag in a Grignard section is characterized by comprising the following devices: the Grignard hydrolysis kettle is sequentially connected with a double-cone vacuum dryer, a vacuum pump, a circulating water condenser, a frozen brine condenser and a solvent recovery tank, wherein a control valve is welded at a discharge port at one end of the double-cone vacuum dryer, an orifice plate is welded inside the discharge port, the orifice plate is circular, small holes are uniformly distributed in the orifice plate, and filter cloth is arranged on the orifice plate.
2. The device for recovering the solvent from the magnesium slag in the Grignard section according to claim 1, is characterized in that: the pore plate is arranged at a position 20cm away from the discharge hole of the double-cone vacuum dryer.
3. The device for recovering the solvent from the magnesium slag in the Grignard section according to claim 1, is characterized in that: the control valve is a valve of DN 50.
4. The device for recovering the solvent from the magnesium slag in the Grignard section according to claim 1, is characterized in that: the diameter of the hole on the pore plate is 2 mm.
5. The device for recovering the solvent from the magnesium slag in the Grignard section according to any claim 1, is characterized in that: the control valve is connected with a material pumping pipeline.
6. A method for recovering the solvent in the magnesium slag in the Grignard section by adopting the device as defined in any one of claims 1 to 5, which is characterized by comprising the following steps:
(1) putting the materials in the hydrolysis kettle into a double-cone vacuum drier;
(2) temporarily connecting a discharge port valve at the end of a perforated plate welded on a bipyramid vacuum dryer with an intermediate tank by using a movable pipeline, vacuumizing liquid materials in the bipyramid to the intermediate receiving tank, introducing nitrogen gas for protection on a vacuum material pumping pipeline, and removing the pipeline connected with the bipyramid after the material pumping is finished;
(3) opening a vacuum valve on a double-cone vacuum dryer, controlling the pressure to be below-0.086 MPa, introducing hot water at the temperature of 55-80 ℃ into a jacket of the double-cone vacuum dryer, slowly heating, and controlling the temperature in the double-cone vacuum dryer to be 60-70 ℃; simultaneously controlling the temperature of a circulating water condenser and a frozen brine condenser, and keeping the liquid temperature at the outlet of the frozen brine condenser at 0-10 ℃;
(4) and after no obvious distillation exists, opening a discharge port valve at the end of the double-cone unwelded hole plate after drying, pouring out the dried basic magnesium chloride filter residue in the dryer by using a transfer tank, conveying the filter residue to a magnesium residue recovery station for next recovery, and pumping the recovered toluene and tetrahydrofuran solvent to a Grignard section for recycling.
7. The method for recovering the solvent in the magnesium slag in the Grignard section according to claim 6, characterized in that the temperature of the circulating water condenser is controlled to be 20-30 ℃, and the temperature of the chilled brine condenser is controlled to be-5 ℃.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN202011508921.0A CN112619273A (en) | 2020-12-19 | 2020-12-19 | Device and method for recovering solvent from magnesium slag in Grignard section |
| CN202111518963.7A CN114797262B (en) | 2020-12-19 | 2021-12-10 | Device and method for recycling solvent from magnesium slag in Grignard section |
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| CN202011508921.0A CN112619273A (en) | 2020-12-19 | 2020-12-19 | Device and method for recovering solvent from magnesium slag in Grignard section |
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| CN202111518963.7A Active CN114797262B (en) | 2020-12-19 | 2021-12-10 | Device and method for recycling solvent from magnesium slag in Grignard section |
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Citations (4)
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| CN203068928U (en) * | 2012-10-10 | 2013-07-17 | 长沙理工大学 | High-efficient mass-transfer bipyramidal rotary vacuum drier |
| CN203731813U (en) * | 2014-02-26 | 2014-07-23 | 中国石油化工股份有限公司 | Catalyst drying machine |
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| EP3302092A1 (en) * | 2015-06-04 | 2018-04-11 | Advance International, Inc. | Improved methods and systems for recovering protein powder and natural omega-3 oil from animal tissue |
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| CN101638400B (en) * | 2009-08-26 | 2011-11-30 | 上海益民化工有限公司 | Method for recovering tetrahydrofuran from Grignard reaction waste residue of magnesium chloride |
| CN101949638B (en) * | 2010-09-26 | 2011-12-28 | 常州力马干燥工程有限公司 | Double-cone rotary vacuum drying and solvent recovering system |
| CN202304276U (en) * | 2011-11-08 | 2012-07-04 | 平顶山易成新材料股份有限公司 | Vacuum dehydration barrel for silicon carbide powder |
| CN203048826U (en) * | 2012-11-22 | 2013-07-10 | 贵州久联民爆器材发展股份有限公司 | Suction filtering, drying and explosive containing tray used for production of primary explosives |
| CN206891074U (en) * | 2017-07-04 | 2018-01-16 | 江西升华新材料有限公司 | Double conic rotary vacuum dryer and material handling system |
| CN109453554A (en) * | 2018-11-28 | 2019-03-12 | 黄石法姆药业股份有限公司 | A kind of drainage pad on centrifugation nutsch filter |
| CN109535113A (en) * | 2018-12-10 | 2019-03-29 | 安徽金禾实业股份有限公司 | A kind of maltol lyophilization method and device |
| CN211274647U (en) * | 2019-11-18 | 2020-08-18 | 广东省肇庆华格生物科技有限公司 | Two-phase separator of ethyl maltol grignard hydrolysis |
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2020
- 2020-12-19 CN CN202011508921.0A patent/CN112619273A/en active Pending
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- 2021-12-10 CN CN202111518963.7A patent/CN114797262B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203068928U (en) * | 2012-10-10 | 2013-07-17 | 长沙理工大学 | High-efficient mass-transfer bipyramidal rotary vacuum drier |
| CN203731813U (en) * | 2014-02-26 | 2014-07-23 | 中国石油化工股份有限公司 | Catalyst drying machine |
| CN204034374U (en) * | 2014-08-11 | 2014-12-24 | 广东省肇庆香料厂有限公司 | A kind of multifunctional vacuum Suction filtration device |
| EP3302092A1 (en) * | 2015-06-04 | 2018-04-11 | Advance International, Inc. | Improved methods and systems for recovering protein powder and natural omega-3 oil from animal tissue |
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| CN114797262B (en) | 2024-03-29 |
| CN114797262A (en) | 2022-07-29 |
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Application publication date: 20210409 |