Catalyst separation device in oxalate production process

Abstract

The utility model belongs to the technical field of chemical engineering, and particularly relates to a catalyst separation device in the production process of oxalate. Comprising a filter; the filter is connected with a backwashing tank; compared with the prior art, the backwashing equipment is added on the basis of the filter, the connection mode of the filter and various materials is improved, a catalyst enters the filter from bottom to top and penetrates through the filter element from inside to outside to be filtered, and the filtering effect of the catalyst is further improved. The catalyst can be concentrated and recycled, and the purposes of recycling and cyclic utilization of the catalyst are achieved. In addition, the catalyst separation device has the characteristics of high efficiency, energy conservation, small occupied area, short flow, easiness in operation and the like.

Description

TECHNICAL FIELD

[0001] The utility model belongs to chemical technology field, concretely relates to a catalyst separation device in oxalate production process. BACKGROUND

[0002] Oxalate is a kind of organic compound, and it contains oxalic acid group (-COO-) and hydrocarbon compound to form ester by esterification reaction in molecule. The synthesis of oxalate is very important in chemical industry, and it is the key intermediate of synthesizing oxalic acid and other chemicals, and is widely used in preparing dye, medicine, solvent, extractant and intermediate of various chemical products.

[0003] Catalyst separation is one of the key steps in oxalate production process, which directly affects the purity and recovery rate of oxalate. The existing catalyst separation technology in oxalate production process has the following problems: first, the equipment is complex: the traditional catalyst separation equipment, such as the packed tower, has complex structure, high purchase cost, and needs to use packing in the process of use, which not only increases the maintenance difficulty, but also increases the production cost. Second, high energy consumption increases production cost and causes certain burden to the environment. Third, long reaction process leads to low efficiency. Fourth, it is easy to have side reaction, which affects the product quality. Fifth, the catalyst separation is not complete or the separation efficiency is not high, which causes environmental pollution problem. Sixth, the maintenance is complex, which increases the maintenance workload and cost in the later period. SUMMARY

[0004] In order to overcome the defects of the prior art, the utility model provides a catalyst separation device in oxalate production process.

[0005] In order to realize the above-mentioned purpose, the technical scheme of the utility model is as follows: a catalyst separation device in oxalate production process, including filter, the filter is connected with a backwashing tank, the filter is a cylinder, the cylinder top is provided with nitrogen inlet, backwash liquid inlet II, the outer side of the cylinder is provided with backblowing nitrogen port, steam inlet, filtered clear liquid outlet I, filtered clear liquid outlet II, the bottom of the cylinder is provided with backwash liquid inlet I, raw material inlet, filter turbidity liquid outlet, condensate outlet, the inside of the cylinder is equipped with multiple filter elements, backwash liquid inlet I, backwash liquid inlet II are connected with backwashing tank outlet pipeline respectively, the catalyst separation device is also provided with nitrogen inlet pipe, steam inlet pipe, raw material inlet pipe, backwash liquid inlet pipe, filter turbidity liquid outlet pipe, condensate outlet pipe, filtered clear night outlet pipe, nitrogen inlet, backblowing nitrogen port are connected with nitrogen inlet pipe respectively, steam inlet is connected with steam inlet pipe, raw material inlet is connected with raw material inlet pipe, backwash liquid inlet pipe is connected with backwashing tank inlet, filtered clear liquid outlet I, filtered clear liquid outlet II are connected with filtered clear night outlet pipe respectively, condensate outlet is connected with condensate outlet pipe, filter turbidity liquid outlet is connected with filter turbidity liquid outlet pipe. By adopting the production device structure is simple, easy operation.

[0006] The filter element of the catalyst separation device in the oxalate production process is one of a metal membrane filter element and a ceramic membrane filter element.

[0007] The filter of the catalyst separation device in the oxalate production process is at least two, connected in parallel.

[0008] The filter of the catalyst separation device in the oxalate production process is at least two, connected in series.

[0009] The catalyst separation device in the oxalate production process is further provided with a concentration device, and the filter turbid liquid outlet is connected with the concentration device through a filter turbid liquid outlet pipe.

[0010] The catalyst separation device in the oxalate production process is further provided with a security filter, and the filter clear liquid outlet I and the filter clear liquid outlet II are connected with the security filter through pipelines.

[0011] The filter of the catalyst separation device in the oxalate production process is provided with a steam insulation jacket outside.

[0012] The filter of the catalyst separation device in the oxalate production process is a dead-end filter.

[0013] Compared with the prior art, the filter is provided with a backwashing device, and the connection mode of the filter and various materials is improved, the catalyst enters the filter from bottom to top, and is filtered from inside to outside through the filter element, so that the catalyst filtering effect is further improved; through the above-mentioned internal filtering and filter offline backwashing device, catalyst concentration recovery can be realized, the purpose of catalyst recovery and recycling is achieved, nitrogen backblowing and ethanol backwashing can effectively solve the problem of filter element hole blockage, and the catalyst separation device has the advantages of high catalyst separation precision, high separation efficiency and the like. BRIEF DESCRIPTION OF DRAWINGS

[0014] Figure 1The utility model discloses a catalyst separation device process schematic diagram in oxalate production process.

[0015] Figure 2 For Figure 1 Filter schematic diagram.

[0016] Figure 3 For Figure 2 Filter A partial enlarged view.

[0017] Figure 4 The utility model discloses a filter series process schematic diagram in catalyst separation device in oxalate production process described in embodiment 5.

[0018] Figure Figure 5 The utility model discloses a catalyst separation method process schematic diagram in oxalate production process described in embodiment 6-7.

[0019] Figure 6 The utility model discloses a catalyst separation device process schematic diagram in oxalate production process described in embodiment 8-19.

[0020] Figures 1-6 In, 1 is backwash tank, 2 is filter A, 3 is filter B, 4 is cylinder, 5 is steam heat preservation jacket, 6 is filter element, 7 is concentration equipment, 8 is security filter, 9 is filter A', a is nitrogen import pipe, b is steam import pipe, c is raw material import pipe, d is backwash liquid import pipe, e is filter clear liquid export pipe, f is condensate export pipe, g is filter turbid liquid export pipe, h is backwash liquid export pipe, j is concentrated catalyst residue slurry export pipe, k is blow-off pipe;A' is backblowing nitrogen port, a" is nitrogen import, b' is steam import, c' is raw material import, d' is backwash liquid import I, d" is backwash liquid import II, e' is filter clear liquid export I, e" is filter clear liquid export II, f' is condensate export, g' is filter turbid liquid export. DETAILED DESCRIPTION

[0021] Embodiment 1: refer to attached Figures 1-3The embodiment relates to a catalyst separation device in an oxalate production process, comprising a filter 2; the filter is connected with a backwashing tank 1; the filter is a cylinder body 4, the top of the cylinder body is provided with a nitrogen inlet a'', a backwashing liquid inlet II d'', the outer side of the cylinder body is provided with a backblowing nitrogen port a', a steam inlet b', a filtered clear liquid outlet I e', a filtered clear liquid outlet II e'', the bottom of the cylinder body is provided with a backwashing liquid inlet I d', a raw material inlet c', a filtered turbid liquid outlet g' and a condensed liquid outlet f', and a plurality of filtering elements 6 are arranged in the cylinder body; the backwashing liquid inlet I d' and the backwashing liquid inlet II d'' are respectively connected with outlet pipelines of the backwashing tank 1; the catalyst separation device is further provided with a nitrogen inlet pipe a, a steam inlet pipe b, a raw material inlet pipe c, a backwashing liquid inlet pipe d, a filtered turbid liquid outlet pipe g, a condensed liquid outlet pipe f and a filtered clear liquid outlet pipe e; the nitrogen inlet a'' and the backblowing nitrogen port a' are respectively connected with the nitrogen inlet pipe; the steam inlet b' is connected with the steam inlet pipe; the raw material inlet c' is connected with the raw material inlet pipe; the backwashing liquid inlet pipe is connected with the backwashing tank inlet; the filtered clear liquid outlet I e' and the filtered clear liquid outlet II e'' are respectively connected with the filtered clear liquid outlet pipe; the condensed liquid outlet f' is connected with the condensed liquid outlet pipe; and the filtered turbid liquid outlet g' is connected with the filtered turbid liquid outlet pipe.

[0022] Embodiment 2: refer to the attached Figures 1-3 The catalyst separation device in the oxalate production process disclosed by the embodiment is different in that the filtering element 6 is a metal membrane filtering element.

[0023] Embodiment 3: refer to the attached Figures 1-3 The catalyst separation device in the oxalate production process disclosed by the embodiment is different in that the filtering element 6 is a ceramic membrane filtering element.

[0024] Embodiment 4: refer to the attached Figures 1-3 The catalyst separation device in the oxalate production process disclosed by the embodiment is different in that the filter is at least two, and the filter A and the filter B are connected in parallel.

[0025] Embodiment 5: refer to the attached Figures 2-4 The catalyst separation device in the oxalate production process disclosed by the embodiment is different in that the filter is at least two, and the filter A and the filter A' are connected in series.

[0026] Embodiment 6: refer to the attached Figure 5 The catalyst separation device in the oxalate production process disclosed by the embodiment is different in that a concentration device 7 is further arranged, the filtered turbid liquid outlet of the filter 2 is connected with the concentration device 7 through the filtered turbid liquid outlet pipe g, and the concentration device is a concentrator; the concentrator is provided with a backwashing liquid outlet pipe h and a catalyst residue slurry outlet pipe j after concentration.

[0027] Example 7: refer to the attached Figure 5 The catalyst separation device in the oxalate production process of the present embodiment is different in that a concentration device 7 is further provided, the filtered turbid liquid outlet of the filter 2 is connected with the concentration device 7 through a filtered turbid liquid outlet pipe g, and the concentration device is a rectifying column; the rectifying column is provided with a backwash liquid outlet pipe h and a catalyst residue slurry outlet pipe j after concentration.

[0028] Example 8: refer to the attached Figure 6 The catalyst separation device in the oxalate production process of the present embodiment is different in that a safety filter 8 is further provided, the filtered clear liquid outlet Ie' and the filtered clear liquid outlet IIe" of the filter 2 are connected with the safety filter 8 through pipes.

[0029] Example 9: refer to the attached Figures 1-6 The catalyst separation device in the oxalate production process of the present embodiment is different in that a steam insulation jacket is provided outside the filter.

[0030] Example 10: refer to the attached Figures 1-6 The catalyst separation device in the oxalate production process of the present embodiment is different in that the filter is a dead-end filter.

[0031] Example 11: refer to the attached Figures 1-6 The present embodiment relates to a catalyst separation device process in the oxalate production process, which includes raw material filtration and filter offline backwashing steps, and specifically as follows: (1) raw material filtration: the oxalate slurry containing catalyst from the reaction unit in the oxalate production process enters the filter element 6 from the bottom raw material inlet c' of the filter, filters from the inside to the outside through the filter element 6, and the clear liquid is discharged from the filtered clear liquid outlet IIe" at the upper part of the filter, and the catalyst in the slurry is intercepted on the inner surface of the filter element 6 through surface screening; (2) filter offline backwashing: when the differential pressure of the filter element 6 or the filtration time reaches the set value, the filter offline backwashing is carried out: nitrogen is introduced through the nitrogen inlet a" for residual liquid filtration, after filtration, the backwash liquid is introduced into the filter through the backwash tank 1 and the backwash liquid inlet I d' for catalyst washing, the backwash liquid and the oxalate filtrate are discharged after backwashing, nitrogen is introduced again, and the catalyst thick slurry is discharged through the filtered turbid liquid outlet g' to the catalyst preparation unit, and at the same time, the filter element 6 restores the flux and waits for online operation.

[0032] Example 12: refer to the attached Figures 1-6The embodiment relates to a catalyst separation process method in an oxalate production process, which is different from the prior art in that a concentration step is further arranged after an offline backwashing step of a filter, catalyst thick slurry discharged through a filtered turbid liquid outlet g' is separated from part of backwashing liquid through a concentration device, and the catalyst residue slurry after concentration is sent to a catalyst preparation unit through a catalyst residue slurry outlet pipe j.

[0033] Embodiment 13: refer to the attached Figures 1-6 The embodiment relates to a catalyst separation process method in an oxalate production process, which is different from the prior art in that a concentration step is further arranged after an offline backwashing step of a filter, catalyst thick slurry discharged through a filtered turbid liquid outlet g' is separated from part of backwashing liquid through a concentration device, and the catalyst residue slurry after concentration is sent to a catalyst preparation unit through a catalyst residue slurry outlet pipe j.

[0034] The embodiment relates to a catalyst separation process method in an oxalate production process, which is different from the prior art in that a concentration step is further arranged after an offline backwashing step of a filter, catalyst thick slurry discharged through a filtered turbid liquid outlet g' is separated from part of backwashing liquid through a concentration device, and the catalyst residue slurry after concentration is sent to a catalyst preparation unit through a catalyst residue slurry outlet pipe j.

Claims

1. A catalyst separation apparatus in an oxalate production process, characterized by: The filter is connected with a backwashing tank; the filter is a cylinder, the top of the cylinder is provided with a nitrogen inlet, a backwashing liquid inlet II, the outer side of the cylinder is provided with a backblowing nitrogen port, a steam inlet, a filtered clear liquid outlet I, a filtered clear liquid outlet II, the bottom of the cylinder is provided with a backwashing liquid inlet I, a raw material inlet, a filtered turbid liquid outlet, a condensed liquid outlet, and a plurality of filter elements are arranged in the cylinder; the backwashing liquid inlet I and the backwashing liquid inlet II are respectively connected with an outlet pipeline of the backwashing tank; the catalyst separation device is further provided with a nitrogen inlet pipe, a steam inlet pipe, a raw material inlet pipe, a backwashing liquid inlet pipe, a filtered turbid liquid outlet pipe, a condensed liquid outlet pipe and a filtered clear liquid outlet pipe; the nitrogen inlet and the backblowing nitrogen port are respectively connected with the nitrogen inlet pipe; the steam inlet is connected with the steam inlet pipe; the raw material inlet is connected with the raw material inlet pipe; the backwashing liquid inlet pipe is connected with an inlet of the backwashing tank; the filtered clear liquid outlet I and the filtered clear liquid outlet II are respectively connected with the filtered clear liquid outlet pipe; the condensed liquid outlet is connected with the condensed liquid outlet pipe; and the filtered turbid liquid outlet is connected with the filtered turbid liquid outlet pipe.

2. The catalyst separation apparatus in an oxalate production process according to claim 1, characterized by: The filter element is one of a metal membrane filter element and a ceramic membrane filter element.

3. The catalyst separation apparatus in an oxalate production process according to claim 2, characterized by: The filter is at least two, connected in parallel.

4. The catalyst separation apparatus in an oxalate production process according to claim 2, characterized by: The filter is at least two, connected in series.

5. The catalyst separation apparatus in an oxalate production process according to claim 3 or 4, characterized in that: A concentration device is further provided, the filtered turbid liquid outlet of the filter is connected with the concentration device through the filtered turbid liquid outlet pipe, and the concentration device is one of a concentrator and a rectifying tower.

6. The catalyst separation apparatus in an oxalate production process according to claim 5, characterized by: A safety filter is further provided, the filtered clear liquid outlet I and the filtered clear liquid outlet II of the filter are connected with the safety filter through pipelines.

7. The catalyst separation apparatus in an oxalate production process according to claim 6, characterized by: The filter is externally provided with a steam heat preservation jacket.

8. The catalyst separation apparatus in an oxalate production process according to claim 7, characterized by: The filter is a dead-end filter.

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