CN110665258A - Organic solvent column type dehydration refining device - Google Patents

Organic solvent column type dehydration refining device Download PDF

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Publication number
CN110665258A
CN110665258A CN201911146120.1A CN201911146120A CN110665258A CN 110665258 A CN110665258 A CN 110665258A CN 201911146120 A CN201911146120 A CN 201911146120A CN 110665258 A CN110665258 A CN 110665258A
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CN
China
Prior art keywords
way switching
tower
switching valve
communicated
filling
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Pending
Application number
CN201911146120.1A
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Chinese (zh)
Inventor
张善志
陈华法
徐卡特
徐群策
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WENZHOU GUOSHIBANG POLYMER MATERIALS CO Ltd
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WENZHOU GUOSHIBANG POLYMER MATERIALS CO Ltd
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Priority to CN201911146120.1A priority Critical patent/CN110665258A/en
Publication of CN110665258A publication Critical patent/CN110665258A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/0202Separation of non-miscible liquids by ab- or adsorption
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/20Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
    • B01D15/203Equilibration or regeneration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/22Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column

Abstract

The invention relates to an organic solvent column type dehydration refining device, which is characterized in that: comprises at least two packed towers and four three-way switching valves; the filling towers are made of organic glass materials with cylindrical structures, the inner cavities of the filling towers are filled with molecular sieves, and the outer wall of each filling tower is provided with a cooling jacket; the discharge port of the first filling tower is respectively communicated with the condenser and the solution storage tank through a first three-way switching valve, and the discharge port of the second filling tower is respectively communicated with the condenser and the solution storage tank through a second three-way switching valve; the feed inlet of the first filling tower and the feed inlet of the second filling tower are communicated with the outlet of a centrifugal pump through a third three-way switching valve, and the inlet of the centrifugal pump is communicated with a primary distillation solution storage tank; the feed inlet of the first packed tower and the feed inlet of the second packed tower are communicated with the heating device through a fourth three-way switching valve. The organic solvent does not contact with air or a high-temperature environment in the whole process, and the method has the advantages of good molecular sieve regeneration effect, high production efficiency, good safety production performance, low production cost and the like.

Description

Organic solvent column type dehydration refining device
Technical Field
The present invention relates to a dehydration purification apparatus for an organic solvent. The invention is suitable for the industrial dehydration and refining process of mass water-containing organic solvents.
Background
During the process of resin hydration, a large amount of organic solvent, such as polar solvent like acetone, is generated. These polar solvents often participate in the entire synthesis of the resin prepolymer and need to be removed by vacuum after the emulsion is formed, resulting in an aqueous product free of organic solvents.
At present, a dehydration refining process device for polar organic solvents miscible with water generally adopts a packing tower filled with a molecular sieve to connect an explosion-proof oven and a vacuum pump for intermittent treatment so as to remove water from the organic solvents; the molecular sieve is dried at high temperature by an oven to obtain regeneration, or high-temperature drying air is introduced into a packed tower in a vacuum state to carry out regeneration activation of the molecular sieve after adsorption. However, the disadvantages of this batch-wise purification of the aqueous organic solvent are: the regeneration effect of the molecular sieve is poor, the treatment time is long, the production efficiency is low, the moisture in the treated molecular sieve is not sufficiently removed, and the like, so that the molecular sieve is difficult to be widely applied. In addition, in the regeneration process of the molecular sieve, the residual organic solvent is contacted with air and a high-temperature environment, so that fire or explosion accidents are easily caused, and great potential safety hazards exist. Meanwhile, the existing process device has higher manufacturing cost and maintenance cost, increases the product cost, and is also an important reason that the treatment mode is difficult to popularize in most resin manufacturing plants.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the organic solvent column type dehydration refining device which has the advantages of good molecular sieve regeneration effect, high production efficiency, good safety production performance and low production cost.
In order to achieve the above object, the present invention provides an organic solvent column type dehydration refining device, which is characterized in that: comprises at least two packed towers and four three-way switching valves; the filling towers are made of organic glass materials with cylindrical structures, molecular sieves are filled in the inner cavities of the filling towers, the outer wall of each filling tower is provided with a cooling jacket, the upper end of each filling tower is provided with a tower top cover, and the bottom of each filling tower is provided with a feeding hole; the lower end of the cooling jacket is provided with a cooling water inlet, the upper end of the cooling jacket is provided with a cooling water outlet, and the tower top cover is provided with a discharge hole and a sieve plate; the discharge port of the first filling tower is respectively communicated with the condenser and the solution storage tank through a first three-way switching valve, and the discharge port of the second filling tower is respectively communicated with the condenser and the solution storage tank through a second three-way switching valve; the feed inlet of the first filling tower and the feed inlet of the second filling tower are communicated with the outlet of a centrifugal pump through a third three-way switching valve, and the inlet of the centrifugal pump is communicated with a primary distillation solution storage tank; the feed inlet of the first packed tower and the feed inlet of the second packed tower are communicated with the heating device through a fourth three-way switching valve.
In the technical scheme, the heating device consists of a box-type resistance furnace and a steam boiler, the box-type resistance furnace and the steam boiler are communicated with an inlet of an air pressure pump through a three-way switching valve, an outlet of the air pressure pump is communicated with an inlet of a fourth three-way switching valve, and two outlets of the fourth three-way switching valve are respectively communicated with a feeding hole of a first filling tower and a feeding hole of a second filling tower.
In the technical scheme, the type of the molecular sieve is 10x or 13x, the inner diameter of a gap is 9-10 Å, and the filling rate is 500 g/L.
Compared with the prior art, the invention has the beneficial effects that: the method is characterized in that a plurality of cylindrical packed towers filled with molecular sieves are connected in parallel, and an organic solvent is not contacted with air or a high-temperature environment in the whole process, so that the method has the advantages of good molecular sieve regeneration effect, high production efficiency, good safety production performance, low production cost and the like.
Drawings
Fig. 1 is a schematic structural view of the present invention.
In the figure: 1. cooling water outlet, 2, tower top cover, 3, discharge port, 4, sieve plate, 5, first packed tower, 6, second packed tower, 7, first three-way switching valve, 8, second three-way switching valve, 9, condenser, 10, output pipe, 11, solvent storage tank, 12, primary distilled solution storage tank, 13, base, 14, feed inlet, 15, cooling water inlet, 16, fourth three-way switching valve, 17, third three-way switching valve, 18, centrifugal pump, 19, air-pressure pump, 20, three-way switching valve, 21, box-type resistance furnace, 22 and steam boiler.
Detailed Description
The organic solvent column type dehydration and purification apparatus shown in FIG. 1 is characterized in that: comprises at least two packed towers and four three-way switching valves; the filling tower is made of organic glass material with a cylindrical structure and is fixedly arranged on the base 13, the machine glass is transparent, the condition of material treatment can be conveniently observed, the inner cavity is filled with molecular sieves, the outer wall of each filling tower is provided with a cooling jacket, the upper end of each filling tower is provided with a tower top cover 2, and the bottom of each filling tower is provided with a feeding hole 14; the lower end of the cooling jacket is provided with a cooling water inlet 15, the upper end of the cooling jacket is provided with a cooling water outlet 1, the tower top cover 2 is provided with a discharge hole 3 and a sieve plate 4, and the aperture of the sieve plate 4 is smaller than 3 mm; the discharge port 3 of the first packed tower 5 is respectively communicated with a condenser 9 and a solution storage tank 11 through a first three-way switching valve 7, the inlet of the first three-way switching valve 7 is communicated with the discharge port 3 of the first packed tower 5, two outlets are respectively communicated with the condenser 9 and the solution storage tank 11, the inlet of the first three-way switching valve 7 is controlled by a control system to be communicated with one outlet, and the discharge port 3 of the first packed tower 5 is switched to be communicated with the condenser 9 or communicated with the solution storage tank 11; the discharge hole of the second packed tower 6 is respectively communicated with a condenser 8 and a solution storage tank through a second three-way switching valve 8, the inlet of the second three-way switching valve 8 is communicated with the discharge hole of the second packed tower 6, two outlets are respectively communicated with the condenser 9 and the solution storage tank 11, the inlet of the second three-way switching valve 8 is controlled by a control system to be communicated with one of the outlets, and the discharge hole of the second packed tower 6 is switched to be communicated with the condenser 9 or communicated with the solution storage tank 11; the condenser 9 has the functions of cooling and gas-liquid separation, high-temperature waste gas is cooled by the condenser 9 and is subjected to gas-liquid separation, the waste water is conveyed to a waste water treatment tank through an output pipe 10, and the waste gas is conveyed to a waste gas treatment tower through a pipeline; the feed inlet 14 of the first packed tower 5 and the feed inlet of the second packed tower 6 are communicated with the outlet of a centrifugal pump 18 through a third three-way switching valve 17, the inlet of the centrifugal pump 18 is communicated with the primary distillation solution storage tank 12, the solution medium in the primary distillation solution storage tank 12 is input into the first packed tower 5 or the second packed tower 6 through the switching of the third three-way switching valve 17 by the centrifugal pump 18, the inlet of the third three-way switching valve 17 is communicated with the centrifugal pump 18, two outlets are respectively communicated with the feed inlet 14 of the first packed tower 5 and the feed inlet of the second packed tower, and the inlet of the third three-way switching valve 17 is controlled by a control system to be communicated with one outlet; the feed inlet 14 of the first packed column 5 and the feed inlet of the second packed column 6 are communicated with a heating device through a fourth three-way switching valve 16, the inlet of the fourth three-way switching valve 16 is communicated with the heat source output port of the heating device, two outlets are respectively communicated with the feed inlet 14 of the first packed column 5 and the feed inlet of the second packed column 6, and the inlet of the fourth three-way switching valve 16 is controlled by a control system to be communicated with one of the outlets.
The heating device consists of a box-type resistance furnace 21 and a steam boiler 22, the box-type resistance furnace 21 and the steam boiler 22 are communicated with the inlet of an air-pressure pump 19 through a three-way switching valve 20, the outlet of the air-pressure pump 19 is communicated with the inlet of a fourth three-way switching valve 16, and the control system controls the three-way switching valve 20 to communicate the air-pressure pump 19 with the heat source output port of the box-type resistance furnace 21 or the steam boiler 22.
The molecular sieve is 10x or 13x in type, the inner diameter of a gap is 9-10 Å, the filling rate is 500g/L, and the organic solvent passes through the packed tower, so that the molecular sieve can fully adsorb water, a small amount of macromolecular solvent and other impurities.
The first packed tower 5 and the second packed tower 14 and 6 form a parallel structure, and the processing capacity of the whole device can be effectively increased by increasing the number of the packed towers.
The working process is as follows:
the third three-way switching valve 17 is switched to the first packed tower 5, the first three-way switching valve 7 is switched to the solution storage tank 11, the second packed tower 6, the second three-way switching valve 8 and the fourth three-way switching valve 16 are all in a closed state, cooling water is opened, cooling water is input from the cooling water inlet 15, and cooling water flows out from the cooling water outlet 1; the centrifugal pump 18 is started to transfer the primarily distilled aqueous organic solvent from the primary distillation solution storage tank 12 to the first packed column 5, and the first round of adsorption is completed by overflowing the adsorption through the molecular sieve until the solution storage tank 11.
Then, the third three-way switching valve 17 is switched to the second packed column 6, the second three-way switching valve 8 is switched to the solution storage tank 11, the centrifugal pump 18 is actuated to transfer the primarily distilled aqueous organic solvent from the primary distillation solution storage tank 12 to the second packed column 6, and the second round of adsorption is completed by passing the overflow stream through the molecular sieve adsorption until the solution storage tank 11.
While the second round of adsorption is performed, the fourth three-way switching valve 16 is switched to the first packed column 5, the first three-way switching valve 7 is switched to the condenser 9, and the three-way switching valve 20 is switched to the steam boiler 22, so that the regeneration and activation processes of the molecular sieve in the inner cavity of the first packed column 5 are performed. Firstly, start steamingThe steam boiler 22 is started, the air pressure pump 19 is started to deliver high-temperature steam to the first packed tower 5, the molecular sieve in the tower is purged for about 1-2 hours, and the high-temperature steam is about 60-80 hours0C; then the three-way switching valve 20 is switched to a box-type resistance furnace 21, the box-type resistance furnace 21 is started to provide high-temperature dry hot air, and the molecular sieve in the inner cavity of the first filling tower 5 is purged for 2-3 hours; then, the first packed tower 5 is cooled by using cooling water, and the whole processes of organic solvent adsorption and molecular sieve regeneration of the first packed tower 5 are completed.
Similarly, when the second round of adsorption is completed, the fourth three-way switching valve 16 is switched to the second packed column 6, the second three-way switching valve 8 is switched to the condenser 9, and the three-way switching valve 20 is switched to the steam boiler 22, so that the regeneration and activation processes of the molecular sieve in the inner cavity of the second packed column 6 are started. Meanwhile, the first packed tower 5 can start a new round of adsorption and regeneration processes, and thus, the circulation alternative work is formed.

Claims (3)

1. The utility model provides an organic solvent column type dehydration refining plant which characterized by: comprises at least two packed towers and four three-way switching valves; the filling towers are made of organic glass materials with cylindrical structures, molecular sieves are filled in inner cavities of the filling towers, the outer wall of each filling tower is provided with a cooling jacket, the upper end of each filling tower is provided with a tower top cover (2), and the bottom of each filling tower is provided with a feeding hole (14); the lower end of the cooling jacket is provided with a cooling water inlet (15), the upper end of the cooling jacket is provided with a cooling water outlet (1), and the tower top cover (2) is provided with a discharge hole (3) and a sieve plate (4); a discharge port (3) of the first filling tower (5) is respectively communicated with a condenser (9) and a solution storage tank (11) through a first three-way switching valve (7), and a discharge port of the second filling tower (6) is respectively communicated with the condenser (8) and the solution storage tank (11) through a second three-way switching valve (8); the feed inlet (14) of the first packed tower (5) and the feed inlet of the second packed tower (6) are communicated with the outlet of a centrifugal pump (18) through a third three-way switching valve (17), and the inlet of the centrifugal pump (18) is communicated with a primary distillation solution storage tank (12); the feed inlet (14) of the first packed column (5) and the feed inlet of the second packed column (6) are communicated with a heating device through a fourth three-way switching valve (16).
2. The column type dehydration and purification apparatus for organic solvent according to claim 1, wherein: the heating device consists of a box-type resistance furnace (21) and a steam boiler (22), the box-type resistance furnace (21) and the steam boiler (22) are communicated with an inlet of an air-pressure pump (19) through a three-way switching valve (20), and an outlet of the air-pressure pump (19) is communicated with an inlet of a fourth three-way switching valve (16).
3. The column type dehydration and purification apparatus of claim 1 or 2, wherein said molecular sieve is of 10x or 13x type, and has an inner diameter of a gap of 9 to 10 Å and a packing ratio of 500 g/L.
CN201911146120.1A 2019-11-21 2019-11-21 Organic solvent column type dehydration refining device Pending CN110665258A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113274763A (en) * 2021-06-08 2021-08-20 清华大学深圳国际研究生院 Method and device for concentrating graphene oxide dispersion liquid

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5271842A (en) * 1991-12-10 1993-12-21 Pall Corporation Contaminant removal system and process
CN203060888U (en) * 2013-02-19 2013-07-17 西安超滤化工有限责任公司 Methylal deep dehydration purifying device
CN205235696U (en) * 2015-12-24 2016-05-18 西安超滤环保科技股份有限公司 Wave energy regenerative molecular sieve dewatering equipment
CN106606889A (en) * 2015-10-22 2017-05-03 浙江诚信医化设备有限公司 Molecular sieve dehydration process and molecular sieve dehydration apparatus
CN109045925A (en) * 2018-08-17 2018-12-21 青岛大拇指环境工程有限公司 A kind of VOCs waste gas recovery processing unit and method
CN211245625U (en) * 2019-11-21 2020-08-14 温州国仕邦高分子材料有限公司 Organic solvent column type dehydration refining device

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5271842A (en) * 1991-12-10 1993-12-21 Pall Corporation Contaminant removal system and process
CN203060888U (en) * 2013-02-19 2013-07-17 西安超滤化工有限责任公司 Methylal deep dehydration purifying device
CN106606889A (en) * 2015-10-22 2017-05-03 浙江诚信医化设备有限公司 Molecular sieve dehydration process and molecular sieve dehydration apparatus
CN205235696U (en) * 2015-12-24 2016-05-18 西安超滤环保科技股份有限公司 Wave energy regenerative molecular sieve dewatering equipment
CN109045925A (en) * 2018-08-17 2018-12-21 青岛大拇指环境工程有限公司 A kind of VOCs waste gas recovery processing unit and method
CN211245625U (en) * 2019-11-21 2020-08-14 温州国仕邦高分子材料有限公司 Organic solvent column type dehydration refining device

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113274763A (en) * 2021-06-08 2021-08-20 清华大学深圳国际研究生院 Method and device for concentrating graphene oxide dispersion liquid

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