CN111359253A - Oxalic acid double-stage vacuum continuous cooling crystallizer - Google Patents
Oxalic acid double-stage vacuum continuous cooling crystallizer Download PDFInfo
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- CN111359253A CN111359253A CN202010311589.2A CN202010311589A CN111359253A CN 111359253 A CN111359253 A CN 111359253A CN 202010311589 A CN202010311589 A CN 202010311589A CN 111359253 A CN111359253 A CN 111359253A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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Abstract
The invention provides an oxalic acid double-stage vacuum continuous cooling crystallizer. The oxalic acid double-stage vacuum continuous cooling crystallizer comprises a first-stage crystallizer; the slurry pump is connected with the primary crystallizer through a pipeline; the secondary crystallizer is connected with the slurry pump through a pipeline; the discharge pump is connected with the secondary crystallizer through a pipeline; the slurry barrel is connected with the discharge pump through a pipeline; the centrifugal separator is connected with the slurry barrel through a pipeline; the mother liquid barrel is connected with the centrifugal separator through a pipeline; the first mother liquid pump is connected with the mother liquid barrel through a pipeline. The two-stage vacuum continuous cooling crystallizer for oxalic acid provided by the invention has the advantages of short crystallization period, large crystal size, high product purity, attractive appearance, high crystallization capacity and low energy consumption.
Description
Technical Field
The invention relates to the field of cooling crystallization, in particular to an oxalic acid double-stage vacuum continuous cooling crystallizer.
Background
The particle size distribution of oxalic acid generally refers to the proportion of particles of a certain particle size or a range of particle sizes that make up the entire crystal. It can be expressed in simple tabular, graphical and functional forms as the distribution of particle sizes of the particle groups. The particle size, particle size distribution and shape of the particles can significantly affect the properties and uses of the magma and its products. In order to master the working condition of the production line and whether the product is qualified, sampling must be carried out on time in the production process, the product is checked for the particle size distribution, and the particle size is required to be measured by crushing and grading. There are various particle size measuring methods, and commonly used are a sieve analysis method, a sedimentation method, a laser method, a small-hole passage method, an adsorption method, and the like. The experiment used a sieve analysis method to determine the crystal size distribution. The sieve analysis method is the simplest and most widely used particle size determination method, and by using the sieve analysis method, not only the particle size distribution can be determined, but also the average particle size at 50% cumulative yield can be obtained by plotting a cumulative particle size characteristic curve. The experiment measures the crystal granularity by a screening method, and aims to:
1. understanding the principle and method of the sieve analysis method for measuring the crystal particle size distribution;
2. and drawing a particle size cumulative distribution curve and a frequency distribution curve according to the sieve analysis data.
At present, the particle size and distribution detection of oxalic acid has no national standard, and the detection standard is established according to a detection office method of similar products and applied as an industrial standard.
Disclosure of Invention
The invention aims to provide the two-stage vacuum continuous oxalic acid cooling crystallizer which has the advantages of short crystallization period, large crystal size, high product purity, attractive appearance, high crystallization capacity and low energy consumption.
In order to solve the technical problem, the two-stage vacuum continuous cooling crystallizer for oxalic acid provided by the invention comprises: a primary crystallizer;
the slurry pump is connected with the primary crystallizer through a pipeline;
the secondary crystallizer is connected with the slurry pump through a pipeline;
the discharge pump is connected with the secondary crystallizer through a pipeline;
the slurry barrel is connected with the discharge pump through a pipeline;
the centrifugal separator is connected with the slurry barrel through a pipeline;
the mother liquid barrel is connected with the centrifugal separator through a pipeline;
the first mother liquid pump is connected with the mother liquid barrel through a pipeline;
the second mother liquor pump is respectively connected with the secondary crystallizer and the mother liquor barrel through pipelines;
the first condenser is connected with the primary crystallizer through a pipeline;
the second condenser is connected with the secondary crystallizer through a pipeline;
and the condensation water bucket is respectively connected with the first condenser and the second condenser through pipelines.
Preferably, a first vertical axial-flow pump and a second vertical axial-flow pump are respectively installed at the bottom sides of the primary crystallizer and the secondary crystallizer.
Preferably, the first condenser is connected with a first liquid ring vacuum unit, and the second condenser is provided with a second liquid ring vacuum unit.
Preferably, the first condenser and the second condenser respectively condense steam generated in the primary crystallizer and the secondary condenser to obtain condensed water, the condensed water is introduced into a condensed water bucket, one side of the condensed water bucket is connected with a first condensed water pump through a pipeline, one side of the first condensed water pump is connected with a second condensed water pump through a pipeline, and the second condensed water pump is respectively connected with the primary crystallizer and the secondary crystallizer through a pipeline.
Preferably, the primary crystallizer is filled with a stock solution, the stock solution is subjected to heat exchange cooling and preliminary crystallization to obtain oxalic acid crystals, a solution containing a certain crystal slurry ratio continuously enters the secondary cooling crystallizer through a slurry pump and is subjected to continuous heat exchange cooling and crystallization to obtain large-particle oxalic acid crystal slurry, the crystal slurry is sent into a slurry barrel through a discharge pump to be stirred, the stirred material is then introduced into a centrifugal separator to be centrifuged, the mother solution obtained after centrifugation is put into a mother solution barrel, and the mother solution in the mother solution barrel is sent to the primary crystallizer through a first mother solution pump for continuous circulation heat exchange crystallization.
Preferably, the first condenser is communicated with cooling water, and the second condenser is communicated with chilled water.
Preferably, the mother liquid barrel is fixedly provided with a support, the support is provided with an air cylinder, a telescopic rod of the air cylinder is provided with a stirring motor, an output shaft of the stirring motor is fixedly provided with a rotating shaft, and the bottom end of the rotating shaft is provided with a stirring blade.
Preferably, the top side of the mother liquid barrel is provided with a feed inlet, the bottom side of the mother liquid barrel is respectively provided with a first discharge outlet and a second discharge outlet, and the first discharge outlet and the second discharge outlet are both provided with a discharge valve.
Compared with the related art, the two-stage vacuum continuous cooling crystallizer for oxalic acid provided by the invention has the following beneficial effects:
the invention provides an oxalic acid two-stage vacuum continuous cooling crystallizer, the two-stage vacuum continuous cooling crystallizer designed by the equipment continuously enters oxalic acid solution which is evaporated and concentrated to 30% concentration and has the temperature of 80 ℃ into the vacuum crystallizer, the temperature is reduced to about 65 ℃ by taking away heat from partial water through flash evaporation, meanwhile, oxalic acid crystals are obtained through preliminary crystallization, the solution containing a certain crystal slurry ratio continuously enters the two-stage crystallizer, large-particle oxalic acid crystal slurry is obtained through continuous heat exchange cooling crystallization, and qualified products are obtained through thick and centrifugal separation of crystals meeting the particle size requirement; the vacuum cooling crystallizer series can be designed into different types and different process flows according to the characteristics of different materials to be treated, and can also be provided with an automatic control system according to the requirements of different users.
The more the number of stages is, the higher the control precision of discharging is, and the yield is higher. The granularity is bigger, helps the sales promotion, satisfies the customer demand that large granularity required.
Drawings
FIG. 1 is a schematic structural view of a two-stage vacuum continuous cooling crystallizer for oxalic acid according to a preferred embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a mother liquid tank in a second embodiment of the two-stage vacuum continuous cooling crystallizer for oxalic acid according to the present invention;
FIG. 3 is a schematic structural diagram of a two-stage vacuum continuous cooling crystallizer for oxalic acid according to a second embodiment of the present invention;
fig. 4 is a schematic structural view of the stirring vane shown in fig. 3.
Reference numbers in the figures: 1. the device comprises a primary crystallizer, a secondary crystallizer, a discharge pump, a slurry barrel, a centrifugal separator, a mother liquor barrel, a mother liquor pump, a vertical axial-flow pump, a centrifugal separator, a condensate tank, a condensate pump, a first condensate pump, a second condensate pump, a bracket, a cylinder, a stirring motor, a rotating shaft, a stirring blade, a feeding port, a first discharge port, a second discharge port, a discharge port, 27, a discharge valve, a mounting seat, a mounting groove, a mounting block, a mounting.
Detailed Description
The invention is further described with reference to the following figures and embodiments.
The first embodiment:
referring to fig. 1, in a first embodiment of the present invention, a two-stage vacuum continuous cooling crystallizer for oxalic acid comprises: a primary crystallizer 1;
the slurry pump 2 is connected with the primary crystallizer 1 through a pipeline;
the secondary crystallizer 3 is connected with the slurry pump 2 through a pipeline;
the discharge pump 4 is connected with the secondary crystallizer 3 through a pipeline;
the slurry barrel 5 is connected with the discharge pump 4 through a pipeline;
the centrifugal separator 6 is connected with the slurry barrel 5 through a pipeline;
the mother liquid barrel 7 is connected with the centrifugal separator 6 through a pipeline 6;
the first mother liquid pump 8 is connected with the mother liquid barrel 7 through a pipeline;
the second mother liquor pump 9, the said second mother liquor pump 9 connects with mother liquor barrel 7 through the pipeline in the two-stage crystallizer 3 separately;
the first condenser 12 is connected with the primary crystallizer 1 through a pipeline;
the second condenser 15 is connected with the secondary crystallizer 3 through a pipeline;
and a condensation water bucket 14, wherein the condensation water bucket 14 is respectively connected with the first condenser 12 and the second condenser 15 through pipelines.
And a first vertical axial-flow pump 10 and a second vertical axial-flow pump 11 are respectively installed at the bottom sides of the primary crystallizer 1 and the secondary crystallizer 3.
The first condenser 12 is connected with a first liquid ring vacuum unit 13, and a second liquid ring vacuum unit 16 is installed on the second condenser 15.
The first condenser 12 and the second condenser 15 respectively condense steam generated in the primary crystallizer 1 and the secondary condenser 3 to obtain condensed water, the condensed water is introduced into the condensed water bucket 14, one side of the condensed water bucket 14 is connected with a first condensed water pump 17 through a pipeline, one side of the first condensed water pump 17 is connected with a second condensed water pump 18 through a pipeline, and the second condensed water pump 18 is respectively connected with the primary crystallizer 1 and the secondary crystallizer 3 through pipelines.
The method comprises the steps of injecting stock solution into a primary crystallizer 1, carrying out heat exchange cooling primary crystallization to obtain oxalic acid crystals, continuously feeding solution containing a certain crystal slurry ratio into a secondary cooling crystallizer 3 through a slurry pump 2, carrying out continuous heat exchange cooling crystallization to obtain large-particle oxalic acid crystal slurry, feeding the crystal slurry into a slurry barrel 5 through a discharge pump 4, stirring, introducing stirred materials into a centrifugal separator 6 for centrifugation, putting mother liquor obtained after centrifugation into a mother liquor barrel 7, and feeding mother liquor in the mother liquor barrel 7 into the primary crystallizer 1 through a first mother liquor pump 8 for continuous circulation heat exchange crystallization.
The first condenser 12 is communicated with cooling water, and the second condenser 15 is communicated with chilled water.
Compared with the related art, the two-stage vacuum continuous cooling crystallizer for oxalic acid provided by the invention has the following beneficial effects:
the invention provides an oxalic acid two-stage vacuum continuous cooling crystallizer, the two-stage vacuum continuous cooling crystallizer designed by the equipment continuously enters oxalic acid solution which is evaporated and concentrated to 30% concentration and has the temperature of 80 ℃ into the vacuum crystallizer, the temperature is reduced to 65 ℃ by taking away heat from partial water through flash evaporation, meanwhile, oxalic acid crystals are obtained through preliminary crystallization, the solution containing a certain crystal slurry ratio continuously enters the two-stage crystallizer, large-particle oxalic acid crystal slurry is obtained through continuous heat exchange cooling crystallization, and qualified products are obtained through thick and centrifugal separation of crystals meeting the particle size requirement; the vacuum cooling crystallizer series can be designed into different types and different process flows according to the characteristics of different materials to be treated, and can also be provided with an automatic control system according to the requirements of different users.
The working principle of the single-stage vacuum continuous cooling crystallizer for oxalic acid provided by the invention is as follows:
when the oxalic acid crystallization device is used, oxalic acid solution which is evaporated and concentrated to be 30% in concentration and 80 ℃ in temperature continuously enters a vacuum crystallizer, heat is taken away through part of water in a flash evaporation mode to enable the temperature to be reduced to 48 ℃, meanwhile, oxalic acid crystals are obtained through primary crystallization, the solution containing a certain crystal slurry ratio continuously enters a cooling crystallizer, large-particle oxalic acid crystal slurry is obtained through continuous heat exchange, cooling and crystallization, and crystals meeting the particle size requirement are thickened and centrifugally separated to obtain qualified products. The method comprises the following specific steps:
1. before starting the machine, compressed air must be started, and all automatic valves of the machine can be opened only by compressed air (the pressure of the compressed air is 0.4-0.8 Mpa);
2. opening all pump mechanical seal cooling water (this step is very important, if the circulation pump mechanical seal can be damaged under the condition of no cooling water, the normal pressure of the circulating water is about 0.2 Mpa);
3. checking and wiping all valves of the equipment, closing all emptying valves and blowdown valves of the equipment, and opening inlet and outlet valves of all pumps;
4. checking the steam pressure, and slowly opening a steam condensate water emptying valve to empty the steam condensate water;
5. turning ON a plastic shell type circuit breaker in a control cabinet, and turning ON a small-sized circuit breaker of a pump and a control power supply circuit breaker which need to be used;
6. clicking a human-computer interface to enter a parameter setting picture, and inputting parameters to be set into a system (such as system operation parameters including a heating temperature set value, a liquid level set value, a pressure set value, a feeding set value and the like);
7. starting pumps connected with cooling water and valves on pipelines, and observing whether the pressure of a cooling water inlet is normal (the normal pressure is about 0.2Mpa, and if the pressure is abnormal, a circulating pump is possibly failed or the valves are not opened);
8. starting the first liquid ring vacuum unit 13, and inspecting whether the equipment has leakage (if the leakage exists, the sound of air suction equipment can be heard);
9. stopping feeding after the material liquid level of the primary crystallizer 1 reaches a set value;
10. after the material circulates in the primary crystallizer 1 for 5 hours, the second liquid ring vacuum unit 16 is started to check whether the equipment has leakage (if the equipment has leakage, the sound of air suction equipment can be heard)
11. When the vacuum degree of the secondary crystallizer 3 is larger than-0.085 Mpa, starting a slurry pump 2 to convey the material to the secondary crystallizer 3, and supplementing the raw material into the primary crystallizer 1;
12. opening a steam stop valve after the material liquid level of the secondary crystallizer 3 reaches a set value;
13. after the material circulates in the secondary crystallizer 3 for 5 hours, the discharging pump 4 is started to convey the material to the slurry barrel 5;
14. starting a mixer of the slurry barrel 5, and opening a discharge valve of the slurry barrel 5 to enable the materials to enter a centrifugal separator 6 for centrifugation;
15. when the equipment is normally produced, the temperature, the vacuum degree, the liquid level and the pressure of the equipment need to be patrolled and examined.
Second embodiment:
based on the two-stage vacuum continuous cooling crystallizer for oxalic acid provided by the first embodiment of the application, the second embodiment of the application provides another two-stage vacuum continuous cooling crystallizer for oxalic acid. The second embodiment is merely a preferred way of the first embodiment, and the implementation of the second embodiment does not affect the implementation of the first embodiment alone.
The second embodiment of the present invention will be further described with reference to the drawings and the following description.
Referring to fig. 2 to 4, the present embodiment is different from the first embodiment in that a support 19 is fixedly installed on the mother liquid tank 7, an air cylinder 20 is installed on the support 19, a stirring motor 21 is installed on a telescopic rod of the air cylinder 20, a rotating shaft 22 is fixedly installed on an output shaft of the stirring motor 21, and a plurality of stirring blades 23 are installed at a bottom end of the rotating shaft 22.
The bottom fixed mounting of pivot 22 has mount pad 28, and a plurality of mounting grooves 29 have been seted up to the annular all around of mount pad 28, and the installation piece 30 is installed to the mounting groove 29 internal rotation, and the one end of installation piece 30 extends to outside the mounting groove 29 and with stirring leaf 23 fixed connection.
A bearing 31 is fixedly arranged in the mounting groove 29, and an inner ring of the bearing 31 is fixedly sleeved with the mounting block 30.
The mounting block 30 is sleeved with a sealing ring 32, and the sealing ring 32 is connected with the inner wall of the mounting groove 29 in a sealing manner.
The top side of the mother liquid barrel 7 is provided with a feeding hole 24, the bottom side of the mother liquid barrel 7 is respectively provided with a first discharging hole 25 and a second discharging hole 26, and the first discharging hole 25 and the second discharging hole 26 are both provided with a discharging valve 27.
The stirring blade 23 of being convenient for reciprocates when rotating the stirring in the stirring process, and stirring effect is better.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. The utility model provides an oxalic acid doublestage vacuum continuous cooling crystallizer which characterized in that includes:
a primary crystallizer;
the slurry pump is connected with the primary crystallizer through a pipeline;
the secondary crystallizer is connected with the slurry pump through a pipeline;
the discharge pump is connected with the secondary crystallizer through a pipeline;
the slurry barrel is connected with the discharge pump through a pipeline;
the centrifugal separator is connected with the slurry barrel through a pipeline;
the mother liquid barrel is connected with the centrifugal separator through a pipeline;
the first mother liquid pump is connected with the mother liquid barrel through a pipeline;
the second mother liquor pump is respectively connected with the secondary crystallizer and the mother liquor barrel through pipelines;
the first condenser is connected with the primary crystallizer through a pipeline;
the second condenser is connected with the secondary crystallizer through a pipeline;
and the condensation water bucket is respectively connected with the first condenser and the second condenser through pipelines.
2. The two-stage vacuum continuous cooling crystallizer for the oxalic acid according to claim 1, wherein a first vertical axial flow pump and a second vertical axial flow pump are respectively installed at the bottom sides of the primary crystallizer and the secondary crystallizer.
3. The two-stage vacuum continuous cooling crystallizer for oxalic acid according to claim 1, wherein the first condenser is connected with a first liquid ring vacuum unit, and the second condenser is provided with a second liquid ring vacuum unit.
4. The two-stage vacuum continuous cooling crystallizer for the oxalic acid according to claim 1, wherein the first condenser and the second condenser respectively condense the steam generated in the first stage crystallizer and the second stage condenser to obtain condensed water, the condensed water is introduced into a condensed water bucket, one side of the condensed water bucket is connected with a first condensed water pump through a pipeline, one side of the first condensed water pump is connected with a second condensed water pump through a pipeline, and the second condensed water pump is respectively connected with the first stage crystallizer and the second stage crystallizer through a pipeline.
5. The two-stage vacuum continuous cooling crystallizer for oxalic acid according to claim 1, wherein a stirring device is installed in the slurry barrel.
6. The two-stage vacuum continuous cooling crystallizer for oxalic acid according to claim 1, wherein the primary crystallizer is filled with a stock solution, and the stock solution is subjected to heat exchange cooling preliminary crystallization to obtain oxalic acid crystals, then a slurry pump is used to continuously feed a solution containing a certain ratio of slurry into the secondary cooling crystallizer, and the solution is subjected to continuous heat exchange cooling crystallization to obtain large-particle oxalic acid crystal slurry, a discharge pump is used to feed the crystal slurry into a slurry barrel for stirring, the stirred material is fed into a centrifugal separator for centrifugation, the mother solution obtained after centrifugation is fed into a mother solution barrel, and then the mother solution in the mother solution barrel is fed into the primary crystallizer by a first mother solution pump for continuous circulation heat exchange crystallization.
7. The two-stage vacuum continuous cooling crystallizer for oxalic acid according to claim 1, wherein the first condenser is communicated with cooling water, and the second condenser is communicated with chilled water.
8. The two-stage vacuum continuous cooling crystallizer for oxalic acid according to claim 1, wherein a support is fixedly installed on the mother liquor barrel, a cylinder is installed on the support, a stirring motor is installed on a telescopic rod of the cylinder, a rotating shaft is fixedly installed on an output shaft of the stirring motor, and a plurality of stirring blades are installed at the bottom end of the rotating shaft.
9. The two-stage vacuum continuous cooling crystallizer for oxalic acid according to claim 8, wherein the bottom end of the rotating shaft is fixedly provided with a mounting seat, the periphery of the mounting seat is annularly provided with a plurality of mounting grooves, a mounting block is rotatably mounted in the mounting groove, one end of the mounting block extends out of the mounting groove and is fixedly connected with the stirring blades, a bearing is fixedly mounted in the mounting groove, the inner ring of the bearing is fixedly sleeved with the mounting block, the mounting block is sleeved with a sealing ring, and the sealing ring is hermetically connected with the inner wall of the mounting groove.
10. The two-stage vacuum continuous cooling crystallizer for oxalic acid according to claim 1, wherein the top side of the mother liquid barrel is provided with a feeding hole, the bottom side of the mother liquid barrel is provided with a first discharging hole and a second discharging hole, and the first discharging hole and the second discharging hole are both provided with a discharging valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202010311589.2A CN111359253A (en) | 2020-04-20 | 2020-04-20 | Oxalic acid double-stage vacuum continuous cooling crystallizer |
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| CN202010311589.2A CN111359253A (en) | 2020-04-20 | 2020-04-20 | Oxalic acid double-stage vacuum continuous cooling crystallizer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112274964A (en) * | 2020-11-18 | 2021-01-29 | 广州市心德实业有限公司 | Ammonium chloride salt slurry cooling crystallization device and cooling crystallization method thereof |
| CN115487529A (en) * | 2022-09-15 | 2022-12-20 | 山东金宜善新材料有限公司 | Circulation crystallization equipment is used in tetrabromobisphenol A production |
-
2020
- 2020-04-20 CN CN202010311589.2A patent/CN111359253A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112274964A (en) * | 2020-11-18 | 2021-01-29 | 广州市心德实业有限公司 | Ammonium chloride salt slurry cooling crystallization device and cooling crystallization method thereof |
| CN112274964B (en) * | 2020-11-18 | 2023-08-25 | 广州市心德实业有限公司 | Ammonium chloride salt slurry cooling crystallization device and cooling crystallization method thereof |
| CN115487529A (en) * | 2022-09-15 | 2022-12-20 | 山东金宜善新材料有限公司 | Circulation crystallization equipment is used in tetrabromobisphenol A production |
| CN115487529B (en) * | 2022-09-15 | 2023-09-12 | 山东金宜善新材料有限公司 | Circulation crystallization equipment is used in tetrabromobisphenol A production |
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