CN211514462U - Gas-liquid continuous reaction device - Google Patents
Gas-liquid continuous reaction device Download PDFInfo
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- CN211514462U CN211514462U CN201922401254.5U CN201922401254U CN211514462U CN 211514462 U CN211514462 U CN 211514462U CN 201922401254 U CN201922401254 U CN 201922401254U CN 211514462 U CN211514462 U CN 211514462U
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Abstract
The utility model discloses a gas-liquid continuous reaction device, which comprises a feed liquid kettle, a reaction tower, a reaction liquid buffer kettle and a reaction liquid kettle; a partition plate is arranged in the reaction tower, a packing layer is arranged on the partition plate, a feeding cavity is formed between the uppermost packing layer and the top wall of the tower body, a discharging cavity is formed between the lowermost partition plate and the bottom wall of the tower body, and a spray head is arranged in the feeding cavity; the liquid outlet of the material liquid kettle is communicated with the spray header through a material supply pipeline; the discharging cavity is communicated with a liquid inlet of the reaction liquid buffer kettle through a discharging pipeline; a liquid outlet of the reaction liquid buffer kettle is communicated with the spray head and a liquid inlet of the reaction liquid kettle through a liquid conveying pipeline; the reaction liquid kettle is communicated with the reaction liquid buffer kettle through a gas return pipe provided with a gas compressor; the reaction liquid buffer kettle is communicated with the reaction tower through a gas return pipe; the reaction tower is connected with an air inlet pipe, and the reaction liquid kettle is connected with a liquid discharge pipe. The device can recycle the gas raw materials dissolved in the reaction liquid in continuous production, thereby saving the gas raw materials, reducing the production cost and solving the problem of waste gas treatment.
Description
Technical Field
The utility model relates to a gas-liquid reaction equipment, concretely relates to gas-liquid continuous reaction device.
Background
The gas-liquid two-phase reaction belongs to common chemical reaction, the existing main reaction mode is to blend gas into liquid for reaction, the solubility of the gas in reaction liquid increases along with the increase of pressure and decreases along with the increase of temperature, especially when the pressure increases, the dissolved gas in the liquid is more, if the residual gas in the kettle is directly emptied before the liquid is emptied, the raw material waste is caused, the production cost is increased, the waste gas difficult to treat is generated, the environment-friendly pressure is increased, if the gas is not emptied, the liquid is directly emptied, the gas has higher solubility in the liquid, the liquid carries more gas raw materials to be discharged out of the kettle, the pressure of the liquid is changed into normal pressure, the pressure is reduced, the gas solubility is reduced, the liquid overflows from the kettle, the waste of the gas raw materials is caused, the production cost is increased, the waste gas difficult to treat is generated, and the environment-.
In the device disclosed in the chinese patent publication No. 106512892B, the discharge pipe and the circulation feed inlet are separately provided, so that continuous feeding and rapid separation can be realized, and the production efficiency can be improved; the contact time can be prolonged, the contact area can be increased, the gas-liquid flash reaction is sufficient, and the quality of the separated materials is guaranteed. However, before the reaction liquid of the device is discharged, the high pressure is maintained in the device all the time, so that a large amount of gas raw materials are dissolved in the reaction liquid, after the reaction liquid is discharged from the device, more gas can be carried, the pressure is changed from the pressure to the normal pressure, the pressure is reduced, the gas solubility is reduced, the gas overflows from the reaction liquid, the waste of the gas raw materials is caused, the production cost is increased, the waste gas which is difficult to treat is generated, and the environmental protection pressure is increased.
Disclosure of Invention
The to-be-solved technical problem of the utility model is not enough to above-mentioned prior art exists, provides a gas-liquid continuous reaction device to reach the purpose of gaseous raw materials, reduction in production cost and the emission that reduces waste gas in the recycle reaction back feed liquid.
In order to solve the technical problem, the utility model provides a gas-liquid continuous reaction device with the following structure, which comprises a feed liquid kettle, a reaction tower, a reaction liquid buffer kettle and a reaction liquid kettle;
the reaction tower comprises a tower body, a plurality of perforated partition plates are arranged in the tower body at intervals up and down, packing layers are arranged on the partition plates, a feeding cavity is formed between the uppermost packing layer and the top wall of the tower body, a discharging cavity is formed between the lowermost partition plate and the bottom wall of the tower body, and a spray head is arranged in the feeding cavity;
the liquid outlet of the material liquid kettle is communicated with the spray header through a material supply pipeline; the discharging cavity is communicated with a liquid inlet of the reaction liquid buffer kettle through a discharging pipeline; the liquid outlet of the reaction liquid buffer kettle is communicated with the spray head and the liquid inlet of the reaction liquid kettle through a liquid conveying pipeline; the reaction liquid kettle is communicated with the reaction liquid buffer kettle through a gas return pipe provided with a gas compressor; the reaction liquid buffer kettle is communicated with the reaction tower through a gas return pipe; the reaction tower is communicated with an air inlet pipe, and the reaction liquid kettle is communicated with a liquid discharge pipe.
And the reaction tower, the reaction liquid buffer kettle and the reaction liquid kettle are respectively connected with an emptying pipe provided with an emptying valve.
The emptying pipe is connected with an air suction device.
The feed pipeline is equipped with the feed pump including the liquid outlet of intercommunication feed liquid cauldron and the feed pipe of shower head on the feed pipe, be equipped with the bleeder valve and the pan feeding valve that are located the feed pump both sides respectively on the feed pipe.
The discharging pipeline comprises a discharging pipe which is communicated with the discharging cavity and the liquid inlet of the reaction liquid buffer kettle, and a discharging valve is connected to the discharging pipe.
And the discharge pipe is connected with a sampling pipe which is connected with a sampling valve in series.
The infusion pipeline comprises an infusion pipe for communicating a liquid outlet of the reaction liquid buffer kettle with a liquid inlet of the reaction liquid kettle, the infusion pipe is connected with an infusion valve, an infusion pump and a liquid inlet valve in series, the infusion valve is positioned between the infusion pump and the reaction liquid buffer kettle, and the liquid inlet valve is positioned between the infusion pump and the reaction liquid kettle; the pipe section of the infusion pipe between the infusion pump and the liquid inlet valve is communicated with the spray head through a liquid return pipe which is connected with a liquid return valve in series.
And a liquid discharge valve and a liquid discharge pump are connected to a liquid discharge pipe of the reaction liquid kettle.
And the gas inlet pipe of the reaction tower is connected with a gas raw material supply device.
The utility model discloses in sending into liquid raw material and gaseous raw materials into the reaction tower in succession with liquid raw materials through feed pipeline and intake pipe, let liquid raw materials and gaseous raw materials react, the reaction liquid that the reaction produced flows into reaction liquid buffering cauldron, reaction liquid among the reaction liquid buffering cauldron is delivered to the reaction liquid cauldron through the infusion pipeline, pressure reduction in the feed liquid cauldron under the gas compressor suction, the gas raw materials that dissolve in the reaction liquid will spill over and is delivered to reaction liquid buffering cauldron by gas compressor, continue to participate in the reaction in the gas return pipe flow income reaction tower again, contain trace and do not contain gaseous raw materials even in the reaction liquid of follow reaction liquid cauldron exhaust. Therefore, the utility model discloses can carry out recycle to dissolving into gaseous raw materials in the reaction liquid in the production process of serialization, both practiced thrift gaseous raw materials, reduced manufacturing cost, solved the difficult problem that increases with environmental protection pressure of exhaust-gas treatment again.
Drawings
The following detailed description of embodiments of the present invention is provided with reference to the accompanying drawings:
fig. 1 is a schematic structural diagram of the present invention.
Detailed Description
Referring to fig. 1, the gas-liquid continuous reaction device provided by the present invention comprises a material liquid kettle 50, a reaction tower 51, a reaction liquid buffer kettle 52 and a reaction liquid kettle 53.
The reaction tower 51 comprises a tower body, a plurality of perforated partition plates 54 are arranged in the tower body at intervals up and down, holes in the perforated partition plates 54 are used for gas and liquid to pass through, packing layers 55 are arranged on the partition plates 54, each packing layer 55 is composed of packing materials placed on the partition plates 54, and the packing materials can be Raschig rings or pall rings or other common chemical packing materials. A feeding cavity 56 is arranged between the packing layer 55 at the top and the top wall of the tower body, a discharging cavity 57 is arranged between the partition plate 54 at the bottom and the bottom wall of the tower body, and a spray header 58 is arranged in the feeding cavity 56. The reaction tower 51 is connected with an air inlet pipe 61 communicated with the inner cavity of the reaction tower, the air inlet pipe 61 is positioned above the lowest partition plate 54 and is arranged close to the partition plate, the air inlet pipe 61 is connected with an air inlet valve 77, and the air inlet pipe 61 is connected with a gas raw material supply device 78; the gas raw material is fed into the reaction tower 51 by a gas raw material feeding device, which may be a pressure tank (bottle) for storing the gas raw material or a combination of a gas raw material storage tank and a gas compressor.
The structure of the feed liquid kettle 50, the reaction liquid buffer kettle 52 and the reaction liquid kettle 53 is basically the same as that of the existing reaction kettle, and the feed liquid kettle, the reaction liquid buffer kettle 52 and the reaction liquid kettle 53 all comprise a kettle body, wherein a stirring device capable of stirring materials is arranged in the kettle body, and the kettle body is connected with a temperature detection device capable of detecting the temperature in the kettle, a pressure detection device capable of detecting the pressure in the kettle, and a temperature regulation device capable of heating or cooling the materials in the kettle. The above listed devices are well known to those skilled in the art and are not shown in the figures. That is, the feed liquid tank 50, the reaction liquid buffer tank 52 and the reaction liquid tank 53 are formed by using an existing reaction tank and are provided with some changes, which will be described in the following paragraphs.
With continued reference to fig. 1, the liquid outlet at the bottom of the feed liquid kettle 50 is communicated with the spray header 58 through a feed line; the feeding pipeline comprises a feeding pipe for communicating a liquid outlet at the bottom of the material liquid kettle 50 with the spray header 58, a feeding pump 64 is arranged on the feeding pipe, and a discharge valve 65 and a feeding valve 66 which are respectively positioned at two sides of the feeding pump 64 are arranged on the feeding pipe; the discharge valve 65 is arranged close to a liquid outlet at the bottom of the material liquid kettle 50, and the feed valve 66 is arranged close to the spray header 58; the top of the feed solution tank 50 is provided with a liquid feed inlet fitted with a feed valve 76 through which liquid feed can be fed into the feed solution tank 50.
The discharging cavity 57 is communicated with a liquid inlet of the reaction liquid buffer kettle 52 through a discharging pipeline; the discharging pipeline comprises a discharging pipe communicated with the bottom of the discharging cavity 57 and a liquid inlet at the top of the reaction liquid buffer kettle 52, the position of the liquid inlet at the top of the reaction liquid buffer kettle 52 is lower than the bottom of the discharging cavity 57, and a discharging valve 67 is connected to the discharging pipe. The discharge valves 67 are provided in two, one near the discharge chamber 57 and the other near the reaction solution buffer tank 52. A sampling pipe is connected to the discharge pipe between the two discharge valves 67, and a sampling valve 74 is connected to the sampling pipe in series; the degree of gas-liquid reaction can be sampled and detected through the sampling pipe.
A liquid outlet at the bottom of the reaction liquid buffer kettle 52 is communicated with a spray head 58 and a liquid inlet at the top of the reaction liquid kettle 53 through a liquid conveying pipeline; the infusion pipeline comprises an infusion pipe for communicating a liquid outlet at the bottom of the reaction liquid buffer kettle 52 with a liquid inlet at the top of the reaction liquid kettle 53, the infusion pipe is connected with an infusion valve 68, an infusion pump 69 and a liquid inlet valve 70 in series, the infusion valve 68 is positioned between the infusion pump 69 and the reaction liquid buffer kettle 52, and the liquid inlet valve 70 is positioned between the infusion pump 69 and the reaction liquid kettle 53; the section of the infusion tube between the infusion pump 69 and the liquid inlet valve 70 is communicated with the spray head 58 through a liquid return tube, and the liquid return tube is connected with a liquid return valve 71. The top of the inner cavity of the reaction liquid kettle 53 is communicated with the top of the inner cavity of the reaction liquid buffer kettle 52 through an air return pipe provided with a gas compressor 59, the air return pipe is connected with two air return valves 75, and the two air return valves 75 are respectively arranged at two sides of the gas compressor 59; the top of the inner cavity of the reaction liquid buffer kettle 52 is communicated with the inner cavity of the reaction tower 51 through an air return pipe 60; the communication position of the gas return pipe 60 with the reaction tower 51 is located above and near the lowermost partition plate 54. The bottom of the reaction solution kettle 53 is communicated with a liquid discharge pipe 62; the drain pipe 62 is connected to a drain valve 72 and a drain pump 73, and the reaction solution in the reaction solution tank 53 can be discharged by the drain pump 73.
The tops of the inner cavities of the reaction tower 51, the reaction liquid buffer kettle 52 and the reaction liquid kettle 53 are respectively connected with an emptying pipe, and the emptying pipe is provided with an emptying valve 63. The evacuation pipe is connected with air suction device 79, air suction device can adopt the vacuum pump, before the operation of gas-liquid reaction unit, takes away the air in reaction tower 51, reaction liquid buffer kettle 52 and reaction liquid kettle 53 through air suction device to keep the air and influence the gas-liquid reaction.
The following details the procedure of using the continuous reaction apparatus in connection with the preparation of 1-methyl-4-methylsulfonylbenzene, and refer to FIG. 1; the preparation of 1-methyl-4-methylsulfonylbenzene comprises the following steps:
(1) adding sodium bicarbonate or sodium carbonate and sodium sulfite into water, heating to 40-70 ℃, adding paratoluensulfonyl chloride and a catalyst, then carrying out heat preservation reaction at the temperature of 60-90 ℃, adding activated carbon for decolorization after the reaction is finished, and filtering after the decolorization to obtain a feed liquid; the mass ratio of sodium bicarbonate or sodium carbonate, water, sodium sulfite, paratoluensulfonyl chloride and catalyst is 0.88-1.00:3.50-7.00:0.66-1.0:1.00:0.0002-0.002, and the catalyst is one or the combination of more than two of sodium phosphate, disodium hydrogen phosphate and sodium dihydrogen phosphate;
(2) feeding the feed liquid obtained in the step (1) into a feed liquid kettle 50 through a liquid raw material inlet provided with a feed valve 76 for later use, opening an emptying valve 63 at the tops of a reaction tower 51, a reaction liquid buffer kettle 52 and a reaction liquid kettle 53, and pumping away air in the reaction tower 51, the reaction liquid buffer kettle 52 and the reaction liquid kettle 53 through a suction device 79; the feeding pump 64, the discharging valve 65, the feeding valve 66, the air inlet valve 77 and the gas raw material feeding device 78 are started, the feed liquid and the gas methyl chloride are continuously fed into the reaction tower 51, the methyl chloride and the feed liquid are subjected to continuous reaction under the conditions that the temperature is 70-120 ℃ and the pressure is 0.2-2.0MPa, the reaction liquid generated by the reaction flows into the reaction liquid buffer kettle 52 through the discharging pipe connected with the discharging valve 67, sampling detection is carried out through the sampling pipe connected with the sampling valve 74 in series in the flowing process, if the reaction liquid is unqualified, then the transfusion valve 68, the infusion pump 69, the liquid return valve 71 and the liquid inlet valve 70 are opened, the unqualified reaction liquid is sent back to the reaction tower 51 for continuous reaction until the sampling detection is qualified, the liquid return valve 71 is closed after the reaction liquid is qualified, the liquid inlet valve 70 is opened, the transfusion valve 68 and the infusion pump 69 are kept opened, and the qualified reaction liquid is sent to the reaction liquid kettle 53; starting a gas compressor 59 and a gas return valve 75, enabling the absolute pressure in the reaction liquid kettle 53 to be less than or equal to 0.1Mpa under the suction of the gas compressor 59, enabling the methane chloride dissolved in the reaction liquid to overflow and be sent back to the reaction liquid buffer kettle 52 by the gas compressor 59, and then returning to the reaction tower 51 through a gas return pipe 60 to participate in the reaction, thereby realizing the gas-liquid separation of the reaction liquid and the methane chloride in the reaction liquid kettle and recycling the methane chloride; the whole gas-liquid reaction and the gas-liquid separation can be continuously carried out;
(3) after gas-liquid separation of the reaction liquid in the reaction liquid kettle, opening a liquid discharge valve 72 and a liquid discharge pump 73 to continuously or intermittently output the reaction liquid in the reaction liquid kettle, adding sodium hydroxide into the output reaction liquid at the temperature of 90-95 ℃ and in a stirring state to adjust the pH value of the reaction liquid to 9-12, cooling after the pH adjustment is finished to crystallize and separate out a product in the reaction liquid, carrying out solid-liquid separation to obtain a solid, and washing and drying the solid to obtain the 1-methyl-4-methylsulfonylbenzene. In the continuous production process, certain liquid levels are required to be kept in the reaction liquid buffer kettle 52 and the reaction liquid kettle 53, and particularly, the reaction liquid in the reaction liquid kettle 53 cannot be emptied so as to prevent air from entering; the temperature in the reaction solution buffer tank 52 and the reaction solution tank 53 is maintained at more than 60 ℃ to prevent the product from crystallizing out.
Claims (9)
1. A gas-liquid continuous reaction device is characterized by comprising a material liquid kettle (50), a reaction tower (51), a reaction liquid buffer kettle (52) and a reaction liquid kettle (53);
the reaction tower (51) comprises a tower body, a plurality of perforated partition plates (54) are arranged in the tower body at intervals up and down, packing layers (55) are arranged on the partition plates (54), a feeding cavity (56) is formed between the uppermost packing layer (55) and the top wall of the tower body, a discharging cavity (57) is formed between the lowermost partition plate (54) and the bottom wall of the tower body, and spray headers (58) are arranged in the feeding cavity (56);
a liquid outlet of the material liquid kettle (50) is communicated with the spray header (58) through a material supply pipeline; the discharging cavity (57) is communicated with a liquid inlet of the reaction liquid buffer kettle (52) through a discharging pipeline; a liquid outlet of the reaction liquid buffer kettle (52) is communicated with a spray head (58) and a liquid inlet of the reaction liquid kettle (53) through a liquid conveying pipeline; the reaction liquid kettle (53) is communicated with the reaction liquid buffer kettle (52) through a gas return pipe provided with a gas compressor (59); the reaction liquid buffer kettle (52) is communicated with the reaction tower (51) through a gas return pipe (60); the reaction tower (51) is communicated with an air inlet pipe (61), and the reaction liquid kettle (53) is communicated with a liquid outlet pipe (62).
2. The continuous gas-liquid reactor as claimed in claim 1, wherein the reaction tower (51), the reaction liquid buffer tank (52) and the reaction liquid tank (53) are each connected to an evacuation pipe equipped with an evacuation valve (63).
3. The continuous gas-liquid reactor as claimed in claim 2, wherein said evacuation pipe is connected to a suction device (79).
4. The gas-liquid continuous reaction device according to claim 1, wherein the supply line comprises a supply pipe for connecting the outlet of the feed liquid tank (50) and the shower head (58), the supply pipe is provided with a supply pump (64), and the supply pipe is provided with a discharge valve (65) and a feed valve (66) which are respectively arranged at two sides of the supply pump (64).
5. The continuous gas-liquid reactor as claimed in claim 1, wherein the discharge line comprises a discharge pipe communicating the discharge chamber (57) with the inlet of the reaction solution buffer vessel (52), and a discharge valve (67) is connected to the discharge pipe.
6. The continuous gas-liquid reactor according to claim 5, characterized in that a sampling pipe connected in series with a sampling valve (74) is connected to the discharge pipe.
7. The gas-liquid continuous reaction device according to claim 1, wherein the infusion line comprises an infusion tube communicating the liquid outlet of the reaction liquid buffer vessel (52) with the liquid inlet of the reaction liquid vessel (53), the infusion tube is connected in series with an infusion valve (68), an infusion pump (69) and a liquid inlet valve (70), the infusion valve (68) is positioned between the infusion pump (69) and the reaction liquid buffer vessel (52), and the liquid inlet valve (70) is positioned between the infusion pump (69) and the reaction liquid vessel (53); the pipe section of the infusion pipe, which is positioned between the infusion pump (69) and the liquid inlet valve (70), is communicated with the spray head (58) through a liquid return pipe which is connected with a liquid return valve (71) in series.
8. The continuous gas-liquid reaction apparatus according to claim 1, wherein a drain valve (72) and a drain pump (73) are connected to the drain pipe (62) of the reaction liquid tank (53).
9. The continuous gas-liquid reaction apparatus according to claim 1, wherein the gas feed pipe (61) of the reaction tower (51) is connected to a gas raw material supply means (78).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201922401254.5U CN211514462U (en) | 2019-12-27 | 2019-12-27 | Gas-liquid continuous reaction device |
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| CN201922401254.5U CN211514462U (en) | 2019-12-27 | 2019-12-27 | Gas-liquid continuous reaction device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113774223A (en) * | 2021-09-14 | 2021-12-10 | 超威电源集团有限公司 | Carbonization reaction device and method for waste lead plaster |
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2019
- 2019-12-27 CN CN201922401254.5U patent/CN211514462U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113774223A (en) * | 2021-09-14 | 2021-12-10 | 超威电源集团有限公司 | Carbonization reaction device and method for waste lead plaster |
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