CN210645248U - Device for continuous liquid-solid separation of sulfuric acid solution containing imine series products - Google Patents
Device for continuous liquid-solid separation of sulfuric acid solution containing imine series products Download PDFInfo
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- CN210645248U CN210645248U CN201921288942.9U CN201921288942U CN210645248U CN 210645248 U CN210645248 U CN 210645248U CN 201921288942 U CN201921288942 U CN 201921288942U CN 210645248 U CN210645248 U CN 210645248U
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 150000002466 imines Chemical class 0.000 title claims abstract description 88
- 239000007787 solid Substances 0.000 title claims abstract description 54
- 238000000926 separation method Methods 0.000 title claims description 16
- 239000007788 liquid Substances 0.000 claims abstract description 127
- 239000000243 solution Substances 0.000 claims abstract description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000005406 washing Methods 0.000 claims abstract description 34
- 239000012530 fluid Substances 0.000 claims abstract description 21
- 238000004062 sedimentation Methods 0.000 claims abstract description 15
- 238000010790 dilution Methods 0.000 claims abstract description 11
- 239000012895 dilution Substances 0.000 claims abstract description 11
- 239000000498 cooling water Substances 0.000 claims abstract description 10
- 238000002347 injection Methods 0.000 claims abstract description 7
- 239000007924 injection Substances 0.000 claims abstract description 7
- 239000013505 freshwater Substances 0.000 claims description 13
- 238000007865 diluting Methods 0.000 claims description 5
- 230000005484 gravity Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 77
- 238000000034 method Methods 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- -1 methyl imine Chemical class 0.000 description 8
- 238000006396 nitration reaction Methods 0.000 description 8
- 238000003860 storage Methods 0.000 description 8
- 239000012295 chemical reaction liquid Substances 0.000 description 7
- 239000008399 tap water Substances 0.000 description 7
- 235000020679 tap water Nutrition 0.000 description 7
- 238000003825 pressing Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000011343 solid material Substances 0.000 description 3
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- UOFFEDRAIFYOBS-UHFFFAOYSA-N butan-1-imine Chemical compound CCCC=N UOFFEDRAIFYOBS-UHFFFAOYSA-N 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
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Abstract
The application discloses a device for continuously separating liquid from solid for sulfuric acid solution containing imine series products, which comprises a liquid-liquid ejector, a heat exchanger, a sedimentation type solid-liquid separator and a washer, wherein a liquid inlet of the liquid-liquid ejector is divided into two paths, one path is introduced into the sulfuric acid solution containing the imine series products, and the other path is introduced into dilution water solution; an injection outlet of the liquid-liquid injector is communicated with a middle liquid inlet of the sedimentation type solid-liquid separator through a hot fluid channel of the heat exchanger by a pipeline, and cooling water is introduced into a cold fluid channel of the heat exchanger; the upper part of the settling solid-liquid separator is provided with an overflow outlet, and the bottom outlet of the settling solid-liquid separator is connected with the solid inlet of the washer through a control valve by a pipeline. The device structure can realize continuous washing of imine series products, greatly improves the production efficiency, and can return the diluted water liquid formed after washing the imine series products to the liquid-liquid ejector for repeated use, thereby greatly reducing the water consumption.
Description
Technical Field
The application discloses a device for continuous liquid-solid separation of sulfuric acid solution containing imine series products.
Background
The process flow for producing imine series products, such as methyl imine, is shown in FIG. 3. The operation process comprises the following steps: adding the dried phthalimide into a material storage tank A while stirring 98% concentrated sulfuric acid; and (3) putting 98% concentrated nitric acid into the material storage tank B. And (3) carrying out nitration reaction on the materials in the storage tank A and the storage tank B through the microchannel reactor, and allowing a reaction solution after the nitration reaction to flow out from an outlet of the microchannel reactor, namely the reaction solution obtained by carrying out the nitration reaction to produce the imine series products, wherein the reaction solution is also called a sulfuric acid solution containing the imine series products.
The prior art post-treatment process of sulfuric acid solution containing imine series products generally comprises the following steps: and adding part of water into the reaction solution, and performing dilution and filter pressing (the mass of the water added in the dilution and filter pressing is 1.5-2 times of that of the reaction solution). Because the imine series products can be dissolved in 98% concentrated sulfuric acid, the solubility of imine in the sulfuric acid solution can be reduced along with the reduction of the concentration of sulfuric acid, and therefore, a great amount of imine products are crystallized and separated out in the process of dilution and filter pressing. Diluting and filter-pressing to obtain waste water containing diluted sulfuric acid, nitric acid and impurities, and adding alkali to neutralize so as to obtain waste water containing sulfate, nitrate and impurities. Washing the solid product obtained after dilution and filter pressing with a large amount of water (when a large amount of water is added for washing, the mass of the added water is 15-20 times of that of the reaction solution which is not subjected to post-treatment initially), and drying the washed product to obtain the final imine series product.
However, the above-mentioned process of post-treating sulfuric acid solution containing imine series products has the following disadvantages: at present, the process for washing the precipitated imine series products is indirect washing, and has the defects of large water consumption, frequent operation and large amount of manual operation. The continuous process research on imine series products does not exist in China, and the method is suitable for the continuous production method of imine products. In the prior art, after an imine series product is precipitated in sulfuric acid, the precipitated imine product is usually washed by adopting an intermittent washing mode, and the process has the problems of large washing water consumption, frequent operation and low production efficiency.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects of the prior art, the utility model aims to provide a device for continuous liquid-solid separation of sulfuric acid solution containing imine series products.
The device for continuously separating the liquid from the solid of the sulfuric acid solution containing the imine series products is characterized by comprising a liquid-liquid ejector, a heat exchanger, a sedimentation type solid-liquid separator and a washer arranged below the sedimentation type solid-liquid separator, wherein a liquid inlet of the liquid-liquid ejector is divided into two paths, one path is filled with the sulfuric acid solution containing the imine series products, and the other path is filled with a dilution water solution for diluting the sulfuric acid solution containing the imine series products; an injection outlet of the liquid-liquid injector is communicated with a middle liquid inlet of the sedimentation type solid-liquid separator through a hot fluid channel of the heat exchanger by a pipeline, and cooling water is introduced into a cold fluid channel of the heat exchanger; the upper part of the settling type solid-liquid separator is provided with an overflow outlet, and the bottom outlet of the settling type solid-liquid separator is connected with the solid inlet of the washer through a control valve by a pipeline; mixing and spraying a sulfuric acid solution containing imine series products and a diluted water solution through a liquid-liquid ejector, cooling the mixture through a heat exchanger, allowing the mixture to enter a settling solid-liquid separator for gravity settling, separating out the imine series products, washing the imine series products in a washer, discharging the imine series products, and discharging the diluted sulfuric acid solution through an overflow outlet at the upper part of the settling solid-liquid separator.
The device for continuously separating the liquid from the solid of the sulfuric acid solution containing the imine series products is characterized by also comprising a delivery pump, wherein a washing liquid outlet of a washer is connected with one of liquid inlets of a liquid-liquid ejector through the delivery pump by a pipeline, and a filter screen is arranged at the washing liquid outlet of the washer so as to deliver diluted water liquid into the liquid-liquid ejector and prevent the washed imine series products from entering the liquid-liquid ejector again; and the washer is provided with a fresh water inlet pipe and a washed solid outlet.
The device for continuously separating the liquid from the solid in the sulfuric acid solution containing the imine series products is characterized in that the washer is a tubular cavity which is obliquely arranged, the fresh water liquid inlet pipe is arranged at the upper part of one end with a lower horizontal elevation of the washer, the washed solid outlet is arranged at the lower part of one end with a lower horizontal elevation of the washer, the washing liquid outlet of the washer is arranged at the upper part of one end with a higher horizontal elevation of the washer, and the solid inlet of the washer is arranged at the upper end of the middle part of the washer.
The device for continuously separating the liquid from the solid in the sulfuric acid solution containing the imine series products is characterized in that a plurality of baffles are arranged at intervals in the scrubber along the inclined length direction of the scrubber, the baffles divide the interior of the scrubber into a plurality of sub-chambers, liquid circulation channels are reserved among the upper parts of the sub-chambers, and solid discharge channels are reserved among the lower parts of the sub-chambers; along the upward inclined direction of the washer, the fresh water inlet pipe and the washed solid outlet are respectively arranged at the upper part and the lower part of the first sub-chamber, the lower outlet of each middle sub-chamber is connected with the lower inlet of the next adjacent sub-chamber through a circulating pump by a pipeline, so that the solution in the middle sub-chamber is conveyed towards the next adjacent sub-chamber through the circulating pump; and a washing liquid outlet of the washer is arranged at the upper part of the last sub-chamber.
The device for continuous liquid-solid separation of the sulfuric acid solution containing the imine series products is characterized in that two ends of the side part of the baffle are fixedly connected with the inner walls of two sides of the washer respectively, and a space is reserved between the upper end of the baffle and the inner wall of the upper end of the washer to form a liquid circulation channel; spaces are arranged between the lower ends of the baffles and the inner wall of the lower end of the washer to form the solid discharge channel.
The device for continuously separating the liquid from the solid of the sulfuric acid solution containing the imine series products is characterized in that a sight glass is arranged on a pipeline between an injection outlet of the liquid-liquid injector and the heat exchanger.
A method for continuous liquid-solid separation of sulfuric acid solution containing imine series products is characterized by comprising the following steps:
s1: carrying out nitration reaction to produce a reaction liquid obtained by producing an imine series product, wherein the reaction liquid is a sulfuric acid solution containing the imine series product, the reaction liquid is taken as a raw material, and diluted water liquid discharged from a washing liquid outlet of a washer is mixed and sprayed by a liquid-liquid sprayer, and then enters a hot fluid channel of a heat exchanger, cooling water is introduced into a cold fluid channel of the heat exchanger to carry out heat exchange and temperature reduction on the solution in the hot fluid channel of the heat exchanger, and the solution in the hot fluid channel of the heat exchanger enters a settling solid-liquid separator to carry out gravity settling;
s2: the method comprises the following steps that a sulfuric acid solution diluted by diluted water liquid flows out of an overflow outlet at the upper part of a settling type solid-liquid separator, an imine series product slowly settles to the bottom of the settling type solid-liquid separator, a control valve is opened to enable the imine series product settled to the bottom of the settling type solid-liquid separator to enter a washer, fresh tap water is introduced into the washer through a fresh water inlet pipe, under the operation action of each circulating pump below the washer, the imine series product is fully washed by water in the washer, and the water in the washer returns to a liquid-liquid ejector through a washing liquid outlet, so that the cyclic utilization of the water is realized; the washed imine series products are slowly collected to the lower part of the washer and finally discharged through a washed solid outlet.
The method for continuously separating the liquid from the solid of the sulfuric acid solution containing the imine series products is characterized in that in the step S1, the mass flow ratio of the diluted water solution entering the liquid-liquid ejector to the reaction solution is 2: 1-3: 1; the temperature of the cooling water introduced into the cold fluid channel of the heat exchanger is 20-40 ℃, and preferably 20-30 ℃.
The method for continuous liquid-solid separation of the sulfuric acid solution containing the imine series products is characterized in that in step S1, in the sulfuric acid solution containing the imine series products, the imine series products are at least one of methyl imine, ethyl imine and butyl imine.
The method for continuously separating the liquid from the solid of the sulfuric acid solution containing the imine series products is characterized in that in the step S2, the ratio of the mass flow of tap water introduced into a washer by a fresh water inlet pipe to the mass flow of the solution conveyed by each circulating pump is 1: 1-5.
Compared with the prior art, the beneficial effects of this application lie in:
1) the utility model provides a device that contains sulphuric acid solution serialization liquid-solid separation of imine series product's simple structure, can realize the serialization washing to imine series product through the device structure, production efficiency has been improved greatly, and the running water can return to used repeatedly in the liquid-liquid sprayer again to the dilute water liquid that forms after imine series product washes, the sulphuric acid solution that contains imine series product can emit partial heat after diluting water liquid, gets into after the heat exchanger cooling and subsides in the subside formula solid-liquid separator and separate out the settlement.
2) This application sets up a plurality of baffles in the scrubber, and the scrubber below sets up a plurality of circulating pump, can realize the continuous washing of running water to imine series product through setting up of baffle and circulating pump. Part of sulfuric acid remains on the imine series products, and when tap water washes the imine series products, part of sulfuric acid enters the tap water, so that dilute water liquid containing sulfuric acid is formed. And the scrubber is placed in an inclined mode, the concentration of sulfuric acid in the diluted water liquid in the scrubber is lower and lower along the downward direction of the inclined length of the scrubber, the washing degree of the washed imine series products is higher and higher, the concentration of the imine series products collected at the bottom of the scrubber is higher and higher, and finally the completely washed imine series products are discharged from the lower part of one end with the lower horizontal elevation of the scrubber.
Drawings
FIG. 1 is a schematic structural diagram of a device for continuous liquid-solid separation of sulfuric acid solution containing imine series products;
FIG. 2 is a schematic diagram of the scrubber of the present application;
FIG. 3 is a flow diagram of a prior art process for producing methyl imine;
in the figure: the device comprises a liquid-liquid ejector 1, a viewing mirror 2, a settling solid-liquid separator 3, a control valve 4, a washer 5, a baffle 6, a circulating pump 7, a conveying pump 8, a fresh water inlet pipe 9, a washed solid outlet 10, an overflow outlet 11, a raw material inlet pipe 12, a water inlet pipe 13, a water outlet pipe 14, a heat exchanger 15, a first sub-cavity A and a final sub-cavity B.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
Example (b): refer to FIGS. 1-2
A device for continuous liquid-solid separation of sulfuric acid solution containing imine series products comprises a liquid-liquid ejector 1, a heat exchanger 15, a sedimentation type solid-liquid separator 3, a washer 5 and a delivery pump 8, wherein the washer 5 and the delivery pump 8 are arranged below the sedimentation type solid-liquid separator 3, a liquid inlet of the liquid-liquid ejector 1 is divided into two paths, one path is filled with the sulfuric acid solution containing the imine series products, and the other path is filled with dilution water liquid for diluting the sulfuric acid solution containing the imine series products (compare with figure 1, a raw material liquid inlet pipe 12 for filling the sulfuric acid solution containing the imine series products is arranged on the liquid-liquid ejector 1); an injection outlet of the liquid-liquid injector 1 is communicated with a middle liquid inlet of the sedimentation type solid-liquid separator 3 through a hot fluid channel of a heat exchanger 15 by a pipeline, and cooling water is introduced into a cold fluid channel of the heat exchanger 15; the upper part of the sedimentation type solid-liquid separator 3 is provided with an overflow outlet 11, and the bottom outlet of the sedimentation type solid-liquid separator 3 is connected with the solid inlet of the scrubber 5 through a control valve 4 by a pipeline; the sulfuric acid solution containing imine series products and the diluted water solution are mixed and sprayed out through the liquid-liquid sprayer 1, cooled through the heat exchanger 15, and then enter the settling solid-liquid separator 3 for gravity settling, the imine series products are separated out and washed in the washer 5 and then discharged, and the sulfuric acid solution diluted by the diluted water solution is discharged from the overflow outlet 11 at the upper part of the settling solid-liquid separator 3. And a sight glass 2 is arranged on a pipeline between an injection outlet of the liquid-liquid injector 1 and the heat exchanger 15.
Referring to fig. 1, an inlet of a cold fluid channel of the heat exchanger 15 is connected to a water inlet pipe 13, an outlet of the cold fluid channel of the heat exchanger 15 is connected to a water outlet pipe 14, cooling water is introduced into the cold fluid channel of the heat exchanger 15 through the water inlet pipe 13, and the cooling water after heat exchange flows out from the water outlet pipe 14.
Referring to fig. 2, the scrubber 5 is a tubular chamber disposed obliquely, the fresh water inlet pipe 9 is disposed at the upper portion of the lower end of the horizontal elevation of the scrubber 5, the washing solid outlet 10 is disposed at the lower portion of the lower end of the horizontal elevation of the scrubber 5, the washing liquid outlet 501 of the scrubber 5 is disposed at the upper portion of the higher end of the horizontal elevation of the scrubber 5, and the solid inlet of the scrubber 5 is disposed at the upper end of the middle portion of the scrubber 5.
A plurality of baffles 6 are arranged in the scrubber 5 at intervals along the inclined length direction of the scrubber, and the baffles 6 divide the inside of the scrubber 5 into a plurality of sub-chambers; along the direction that the washer 5 inclines upwards, the fresh water inlet pipe 9 and the washed solid outlet 10 are respectively arranged at the upper part and the lower part of the first sub-chamber A, the lower outlet of each middle sub-chamber is connected with the lower inlet of the next adjacent sub-chamber through a circulating pump 7 by a pipeline, so that the solution in the middle sub-chamber is conveyed towards the next adjacent sub-chamber through the circulating pump 7; a washing liquid outlet 501 of the washer 5 is disposed at the upper portion of the last sub-chamber B.
A plurality of baffles 6 are arranged at intervals in the washer 5, the baffles 6 are arranged to enable the solution to form a vortex in the washer 5, and the solution flows upwards integrally on the basis of the vortex formed in the washer 5. Set up a plurality of circulating pumps 7, further strengthened the intensity of vortex for carry out the abundant washing of material in the baffle. Secondly, the lower part outlet of the middle sub-chamber is connected with the lower part inlet of the next adjacent sub-chamber with higher horizontal elevation through a circulating pump 7 by a pipeline, so that the materials are prevented from being deposited at the bottom of the washer 5, and the circulating conveying through the circulating pump 7 is favorable for washing and mixing the materials and the solution. Although the circulation of the circulation pump 7 is beneficial to the washing and mixing of the material and the solution, along the advancing direction of the last chamber B towards the first chamber a, the sulfuric acid concentration of the solution in the washer 5 is lower and higher, the solid material concentration in the washer 5 is higher and higher, the solid material with high final washing degree is slowly collected in the first chamber a and finally can be discharged from the washed solid outlet 10 (wherein the washed solid outlet 10 is provided with a control valve, and the product is discharged from the washed solid outlet 10 by opening the control valve).
Referring to fig. 1, a washing liquid outlet 501 of the scrubber 5 is connected to one of the liquid inlets of the liquid-liquid ejector 1 through the delivery pump 8, and a filter screen is installed at the washing liquid outlet 501 of the scrubber 5 to deliver dilution water (a solution obtained by washing an imine-series product with tap water in the scrubber 5, referred to as dilution water) into the liquid-liquid ejector 1 and prevent the washed imine-series product from entering the liquid-liquid ejector 1 again.
Referring to fig. 2, both ends of the lateral part of the baffle 6 are fixedly connected with the inner walls of both sides of the washer 5, respectively. A space is reserved between the upper end of the baffle 6 and the inner wall of the upper end of the washer 5 to form a plurality of liquid circulation channels of the sub-chambers in the washer 5. Spaces are arranged between the lower end of the baffle 6 and the inner wall of the lower end of the washer 5 to form a plurality of solid discharge channels of the sub-chambers in the washer 5, and under the action of the solid discharge channels, solid materials in the washer 5 are slowly collected into the first sub-chamber A.
The process for producing the methyl imine by adopting the prior art comprises the following steps: adding 360kg of dried phthalimide into a storage tank A while stirring 150kg of 98% concentrated sulfuric acid; 150kg of 98% concentrated nitric acid is put into the storage tank B. The materials in the material storage tank A and the material storage tank B enter the microchannel reactor at the same mass flow rate to carry out nitration reaction at 65 ℃, and the reaction liquid after nitration reaction flows out from the outlet of the microchannel reactor, namely the reaction liquid obtained by carrying out nitration reaction to produce imine series products, wherein the reaction liquid is also called sulfuric acid solution containing imine series products.
When the device for continuously separating the liquid from the solid of the sulfuric acid solution containing the imine series products is used for continuously separating the liquid from the solid of the sulfuric acid solution containing the imine series products, the device comprises the following processes:
s1: carrying out nitration reaction to produce a reaction solution obtained by producing an imine series product, wherein the reaction solution is a sulfuric acid solution containing the imine series product (the imine series product in the embodiment is methyl imine), mixing and spraying the reaction solution serving as a raw material and a diluted water solution discharged from a washing solution outlet 501 of a washer 5 through a liquid-liquid sprayer 1, feeding the mixed water solution into a hot fluid channel of a heat exchanger 15, simultaneously introducing cooling water into a cold fluid channel of the heat exchanger 15 to carry out heat exchange and temperature reduction on the solution in the hot fluid channel of the heat exchanger 15, and feeding the solution in the hot fluid channel of the heat exchanger 15 into a settling solid-liquid separator 3 to carry out gravity settling;
s2: the sulfuric acid solution diluted by the diluted water solution flows out of an overflow outlet 11 at the upper part of the settling solid-liquid separator 3, the imine series products slowly settle to the bottom of the settling solid-liquid separator 3, the control valve 4 is opened to ensure that the imine series products settled to the bottom of the settling solid-liquid separator 3 enter the washer 5, fresh tap water is introduced into the washer 5 through the fresh water inlet pipe 9, the imine series products are fully washed by the water in the washer 5 under the operation action of each circulating pump 7 below the washer 5, and the water in the washer 5 returns to the liquid-liquid ejector 1 through the washing liquid outlet 501, so that the water is recycled; the washed imine products (i.e. the methyl imine products) are slowly collected at the lower part of the washer 5 and finally discharged through the washed solid outlet 10 (the purity of the methyl imine products discharged from the washed solid outlet 10 is about 95% after being dried).
In step S1, the mass flow ratio of the diluted water liquid entering the liquid-liquid ejector 1 to the reaction liquid is 2.5: 1; the temperature of the cooling water introduced into the cold fluid channel of the heat exchanger 15 is 20-30 ℃.
In step S1, in the sulfuric acid solution containing the imine products, the imine products are at least one of methyl imine, ethyl imine, and butyl imine.
In step S2, the ratio of the mass flow of the tap water introduced into the scrubber 5 by the fresh water inlet pipe 9 to the mass flow of the solution delivered by each circulation pump 7 is 1: 2, and the mass flow of the solution delivered by each circulation pump 7 is large, so that the vortex strength of the solution flowing in the scrubber 5 can be increased to a certain extent.
The description is given for the sake of illustration only, and should not be construed as limiting the scope of the invention to the particular forms set forth in the examples.
Claims (6)
1. A device for continuous liquid-solid separation of sulfuric acid solution containing imine series products is characterized by comprising a liquid-liquid ejector (1), a heat exchanger (15), a sedimentation type solid-liquid separator (3) and a washer (5) arranged below the sedimentation type solid-liquid separator (3), wherein a liquid inlet of the liquid-liquid ejector (1) is divided into two paths, one path is filled with sulfuric acid solution containing imine series products, and the other path is filled with dilution water liquid for diluting the sulfuric acid solution containing imine series products; an injection outlet of the liquid-liquid injector (1) is communicated with a middle liquid inlet of the sedimentation type solid-liquid separator (3) through a hot fluid channel of a heat exchanger (15) by a pipeline, and cooling water is introduced into a cold fluid channel of the heat exchanger (15);
an overflow outlet (11) is arranged at the upper part of the sedimentation type solid-liquid separator (3), and a bottom outlet of the sedimentation type solid-liquid separator (3) is connected with a solid inlet of the scrubber (5) through a control valve (4) by a pipeline; sulfuric acid solution containing imine series products and diluted water solution are mixed and sprayed out through a liquid-liquid sprayer (1), the mixture is cooled through a heat exchanger (15), the mixture enters a settling type solid-liquid separator (3) for gravity settling, the imine series products are separated out and washed in a washer (5) and then discharged, and an overflow outlet (11) at the upper part of the settling type solid-liquid separator (3) discharges the sulfuric acid solution diluted by the diluted water solution.
2. The device for continuous liquid-solid separation of sulfuric acid solution containing imine series products according to claim 1, characterized by further comprising a transfer pump (8), wherein the washing liquid outlet (501) of the scrubber (5) is connected with one of the liquid inlets of the liquid-liquid ejector (1) through the transfer pump (8) by a pipeline, and a filter screen is installed at the washing liquid outlet (501) of the scrubber (5) to transfer dilution water liquid into the liquid-liquid ejector (1) and prevent washed imine series products from reentering the liquid-liquid ejector (1); the washer (5) is provided with a fresh water inlet pipe (9) and a washed solid outlet (10).
3. The apparatus for continuous liquid-solid separation of sulfuric acid solution containing imine series products according to claim 2, wherein the scrubber (5) is a tubular chamber placed obliquely, the fresh water inlet pipe (9) is disposed at the upper part of the end of the scrubber (5) with lower horizontal elevation, the washed solid outlet (10) is disposed at the lower part of the end of the scrubber (5) with lower horizontal elevation, the washing liquid outlet (501) of the scrubber (5) is disposed at the upper part of the end of the scrubber (5) with higher horizontal elevation, and the solid inlet of the scrubber (5) is disposed at the upper middle part of the scrubber (5).
4. The device for continuous liquid-solid separation of sulfuric acid solution containing imine series products according to claim 3, characterized in that a plurality of baffles (6) are arranged at intervals along the inclined length direction inside the scrubber (5), the baffles (6) divide the inside of the scrubber (5) into a plurality of sub-chambers, liquid communication channels are reserved between the upper parts of the sub-chambers, and solid discharge channels are reserved between the lower parts of the sub-chambers; along the direction that the washer (5) inclines upwards, the fresh water inlet pipe (9) and the washed solid outlet (10) are respectively arranged at the upper part and the lower part of the first sub-chamber (A), the lower outlet of each middle sub-chamber is connected with the lower inlet of the next adjacent sub-chamber through a circulating pump (7) by a pipeline, so that the solution in the middle sub-chamber is conveyed towards the next adjacent sub-chamber through the circulating pump (7); and a washing liquid outlet (501) of the washer (5) is arranged at the upper part of the last sub-chamber (B).
5. The device for continuous liquid-solid separation of sulfuric acid solution containing imine series products according to claim 4, wherein two ends of the side of the baffle (6) are fixedly connected with the inner walls of the two sides of the scrubber (5), respectively, and a space is left between the upper end of the baffle (6) and the inner wall of the upper end of the scrubber (5) to form the liquid flow channel; spaces are arranged between the lower end of the baffle (6) and the inner wall of the lower end of the washer (5) to form the solid discharge channel.
6. The device for continuous liquid-solid separation of sulfuric acid solution containing imine series products according to claim 1, characterized in that a sight glass (2) is arranged on a pipeline between the injection outlet of the liquid-liquid injector (1) and the heat exchanger (15).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921288942.9U CN210645248U (en) | 2019-08-09 | 2019-08-09 | Device for continuous liquid-solid separation of sulfuric acid solution containing imine series products |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921288942.9U CN210645248U (en) | 2019-08-09 | 2019-08-09 | Device for continuous liquid-solid separation of sulfuric acid solution containing imine series products |
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| CN210645248U true CN210645248U (en) | 2020-06-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110508038A (en) * | 2019-08-09 | 2019-11-29 | 浙江省天正设计工程有限公司 | A kind of method and device of the sulfuric acid solution serialization solid-liquor separation of the series of products containing imines |
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2019
- 2019-08-09 CN CN201921288942.9U patent/CN210645248U/en not_active Withdrawn - After Issue
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110508038A (en) * | 2019-08-09 | 2019-11-29 | 浙江省天正设计工程有限公司 | A kind of method and device of the sulfuric acid solution serialization solid-liquor separation of the series of products containing imines |
| CN110508038B (en) * | 2019-08-09 | 2024-03-12 | 浙江省天正设计工程有限公司 | Method and device for continuous liquid-solid separation of sulfuric acid solution containing imine series products |
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