CN104107818A - Mobile scar eliminating method of adipic acid crystallizer - Google Patents
Mobile scar eliminating method of adipic acid crystallizer Download PDFInfo
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- CN104107818A CN104107818A CN201410347012.1A CN201410347012A CN104107818A CN 104107818 A CN104107818 A CN 104107818A CN 201410347012 A CN201410347012 A CN 201410347012A CN 104107818 A CN104107818 A CN 104107818A
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- crystallization
- scar
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- adipic acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
- B08B9/093—Cleaning containers, e.g. tanks by the force of jets or sprays
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- Mechanical Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a mobile scar eliminating method of an adipic acid crystallizer. The specific process of the mobile scar elimination comprises the steps of starting movably eliminating scars at a time T0 before the scar elimination is started, wherein the pressure of all crystallizing chambers is P0, i.e. corresponding crystallizing pressure of N chambers; raising the pressure to P1 from P0 at constant speed by a pressure regulating value during the time [delta]T, and raising the temperature of materials in the crystallizing chambers in a balanced way; enabling solution in a part of chambers to achieve an unsaturated state by keeping the pressure P1 for a period of time; gradually dissolving crystal scars; recovering to initial operation from the time T1, wherein the initial operation is the crystallization of N chambers; reducing the pressure to P0 from P1 at constant speed during the time [delta] T, and finishing scar elimination at the time T0+[delta]T. According to the method provided by the invention, the continuity and stability of crystals can be realized, and an aim of energy conservation and emission reduction can be achieved.
Description
Technical field
The present invention relates to a kind of method of the clear scar of crystallizer in adipic acid production.
Background technology
Adipic acid, is commonly called as adipic acid, is loose shape granularity, and wider distribution, has some corrosivity, inflammable, explosive, easily produces static, and excess Temperature is the even rotten a kind of crystalline solid of softening caking easily, 151.9 DEG C of fusing points, 337.5 DEG C of boiling points, 196 DEG C of flash-points.Can there are salt-forming reaction, esterification, amidation process etc. in adipic acid, and can become high molecular polymer etc. with diamine or dihydroxylic alcohols polycondensation.Adipic acid is as a kind of organic synthesis intermediate, be mainly used in synthetic nylon 66 (salt), polyurethane and plasticizer, also can be used for producing senior lubricant, food additives, medicine intermediate, essence and flavoring agent controlling agent, novel monocrystal material, plastics blowing agent, coating, adhesive, pesticide, dyestuff etc.
Crystal system belongs to core process in adipic acid production process.For crystallization of adipic acid technique, its exploitation, to improve, improve what will pay close attention to especially be production capacity, continous-stable and the factor such as energy-conservation of crystallizer.
Crystallization is material with the crystal form of solid from steam, solution, the process of separating out in fused mass.Crystallization of adipic acid technique generally adopts vacuum horizontal multiple-effect evaporation crystallization processes.Vacuum horizontal Multi-effect evaporation crystallizer operating principle is: by its vacuum is controlled in each chamber in crystallizer, each chamber solution adiabatic evaporation under certain vacuum is cooling, concentrated, thereby make solution reach hypersaturated state, the nuclei of crystallization generate and grow up in supersaturated solution.But in crystallizer process, formation adhesion layer easily scabs on equipment wall.These adhesion layers accumulate gradually, be finally full of whole compartment space crystallization can not be carried out again.Therefore need periodically clear scar.
The clear scar method of traditional adipic acid is, each chamber is provided with rinse mouth, and independently carry out each chamber, introduces hot water from the external world, and steam dissolves crystallization of adipic acid.First such design has introduced hot water and steam from the external world, increased intrasystem water content, and because technique finally will obtain crystallized stock, unnecessary water can only be discharged as waste water, has increased the wastewater discharge of technique.Secondly, because crystallization is vacuum evaporating crystalization, unnecessary water adds after system, also needs by vacuum evaporation out, thereby has increased the energy consumption of system.The 3rd, adding of a certain chamber flushing water increases this indoor water content, and crystallization load increases, and is unfavorable for the generation crystallization of continous-stable.
Summary of the invention
The object of the invention is the continous-stable in order to realize crystallization, reach the object of energy-saving and emission-reduction simultaneously.
Technical scheme of the present invention is summarized as follows:
The present invention utilizes the liquid level of crystallizer self, temperature and pressure to regulate, and dissolves and remove the brilliant scar of the inner generation of crystallizer.We claim this method to be called mobile clear scar.Mobile clear scar has various modes, has 11 chambers as example taking crystallizer, and mobile clear scar can be designed with 10 Room crystallizations, 9 Room crystallizations, 8 Room crystallizations, 7 Room crystallizations, 5 Room crystallizations, 4 Room crystallization isotypes.If crystallizer has the individual crystallisation chamber of M (M=7～15, M >=N), under different mode, rear N chamber of whole crystallizer produces crystallization, and front M-N dissolves clear scar in a chamber, and we are referred to as the clear scar of N chamber crystallization this situation.Taking 7 Room crystallizations as example, 7 Room crystallizations represent rear 7 indoor generation crystallizations of crystallizer, and a front M-7 chamber does not produce crystallization, at higher temperature (corresponding higher pressure), the brilliant scar of accumulating are dissolved.
Accompanying drawing 1 is that in the process of mobile clear scar, the pressure of the some chambers of crystallizer changes schematic diagram, before mobile clear scar starts, the pressure of each chamber is P0 (being N the pressure that chamber crystallization is corresponding), the T0 moment starts mobile clear scar, at the uniform velocity rise to P1 by pressure-regulating valve by P0 in Δ T time internal pressure, the now material balance temperature rise of crystallization chamber, then pressure P 1 keeps a period of time, the indoor solution of part reaches undersaturated condition, brilliant scar is dissolved gradually, after brilliant scar has been dissolved, the T1 moment starts to recover to initial operation (being the crystallization of N chamber), in Δ T time internal pressure by P1 uniform descent to P0, the T0+ Δ T moment, clear scar finished.Δ T is inputted by operating personnel.The time that P1 maintains also can be grasped according to the situation that scabs in crystallizer by operating personnel.There are different separately P0 and P1 setting value in each chamber.Each chamber pressure rate of change difference, the time having changed is identical.Δ T span can be set between 10-30min conventionally, and P0 and P1 span can be set between 5mmHgA-400mmHgA according to different chambers.Because the material composition of each chamber is constant, the just physical state of each component changing, under different pressure, temperature when liquid reaches balance is just different, and under different temperatures, the solubility of medium is different, so under different pressures, what the material in different chamber had reaches capacity and output crystallization, and what have does not reach the saturated adipic acid scabbing can being dissolved down, and operating personnel can calculate and determine according to the operational load of each chamber of crystallizer the setup pressure value of each chamber.
Further, above-mentioned crystallizer is also provided with flushing line, can be used as the use of flushing for subsequent use.
The invention has the beneficial effects as follows:
(1), the present invention optimized traditional clear scar mode, cancelled steam and the hot water of the system that enters from the external world.
(2), the present invention is by system itself optimization, reduced system efflux wastewater amount.
(3), owing to adding the discharge reduction of system, make to be reduced by the vacuum evaporation water yield out, thereby reduced the energy consumption of vacuum system.
(4), by the adjusting of crystallizer self system operating parameters, system can be moved continuously, the size of controlled combinations grain.
(5), mobile clear scar method makes crystal system structure simpler, management, easy to maintenance, operating personnel are few.
Brief description of the drawings
Fig. 1 is that crystallizer moves a certain chamber pressure variation of scar schematic diagram clearly
Fig. 2 is the schematic diagram of crystallizer of the present invention.
In figure:
1. crystallizer; 2. pressure-regulating valve; 3. siphon pipe; 4. agitator, 5. outside cleaning hose; 6. vacuum system.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, but do not limit protection scope of the present invention.
Implementation plan 1
As depicted in figs. 1 and 2, the present embodiment has disclosed a kind of clear scar method of movement of crystallization of adipic acid device.
As shown in Figure 2, the crystallizer pattern that adipic acid plant adopts is vacuum horizontal Multi-effect evaporation crystallizer.Crystallizer 1 comprises: pressure-regulating valve 2, siphon pipe 3, agitator 4, outside cleaning hose 5, vacuum system 6.
Crystallizer interior separation is several chambers.When operation, each chamber vacuum difference, increases to last chamber successively from the first Room.Solution of adipic acid transpiring moisture voluntarily under certain vacuum, moisture evaporation absorbs heat, the temperature of solution is reduced successively, thereby solution of adipic acid reaches supersaturation and crystallization.For making the saturation degree of solution even, each indoor agitator that is all provided with of crystallizer, the position of configuration is conducive to supersaturated solution to the flowing of next chamber near siphon pipe part, avoids excessive turbulence and the wearing and tearing of the crystal grain that causes simultaneously.The UNICOM of adjacent two Room realizes by the siphon pipe that is arranged on crystallizer outside.Material, from the first Room charging, passes through each chamber successively by siphon and overflow, obtains the material product of advantages of good crystallization from last chamber.
Although crystallizer inside has adopted polishing, in crystallization process, formation adhesion layer still easily scabs on equipment wall.These adhesion layers accumulate gradually, be finally full of whole compartment space crystallization can not be carried out again.Therefore need periodically clear scar.This cycle will determine according to the speed of the brilliant scar growth of adipic acid in crystallizer, and 2-4 week once conventionally.
Mobile clear scar process is from the T0 moment, staff selects the crystallization of N chamber in the T0 moment, and input Δ T, crystal system starts mobile clear scar process, taking a certain chamber of crystallizer as example, within the Δ T time, this chamber pressure at the uniform velocity rises to P1 by P0, then pressure P 1 keeps a period of time, and brilliant scar is dissolved gradually until the T1 moment is selected the crystallization of M chamber T1 moment staff, in Δ T time internal pressure by P1 uniform descent to P0, the T0+ Δ T moment moves scar clearly and finishes.There are P0 and P1 setting value separately in each chamber.Each chamber pressure rate of change difference, the time having changed is identical.
Taking the crystallizer that formed by 11 chambers as example, under normal circumstances, the each indoor crystallization that produces of crystallizer.The setup parameter of the 11 each chamber of crystallization, Room is as shown in the table, and the vacuum of each chamber increases to last chamber successively from the first Room.Solution of adipic acid is transpiring moisture under certain vacuum, and the temperature of each chamber reduces successively, and the solubility of solution of adipic acid reduces successively, and each chamber all can reach supersaturation and crystallization.In crystallization process, formation adhesion layer still easily scabs on equipment wall.After these adhesion layers run up to a certain degree, staff starts mobile clear scar work.In the time need to removing the brilliant scar of the first two chamber, operating personnel can select 9 Room crystallization patterns, such as the time of mobile clear scar can be given and not fix on 20min not etc., when the time and pattern selected after, the pressure of the each chamber of crystallizer regulates by pressure-regulating valve, 9 Room crystallization pattern downforce setting values are as shown in the table, and in the time of 20min, the force value of each chamber at the uniform velocity changes, the force value of the first two chamber rises, the solution temperature of corresponding each chamber rises, and solubility rises, and scab dissdving is in solution.The pressure of rear Room 7 also respectively has adjusting, makes the variations in temperature of each chamber, and the temperature of last chamber remains unchanged.Change at each chamber pressure after the set point of 9 Room crystallizations, this pressure keeps 30min, and brilliant scar is further dissolved.Reach after 30min when the time, operating personnel reselect 11 Room crystallizations, and the pressure of each chamber is the pressure set points during to 11 Room crystallization in 20min even variation, and crystallizer returns to normal mode of operation.The pattern of mobile clear scar has multiple, and following table is only listed as the setting value of having write under three kinds of patterns, the pressure set points difference under different mode, and the setting-up time of variation is also different, but the principle of the process of mobile clear scar is the same.Reduced steam, hot water and the system efflux wastewater amount of the system that enters by the enforcement of this technology, reduced the energy consumption of system, the system that simultaneously ensured can continuous and steady operation in clear scar process.
Although the preferred embodiments of the present invention are described with preferred embodiment by reference to the accompanying drawings above; but invention is not limited to above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; do not departing from the scope situation that aim of the present invention and claim protect, the equalization of doing changes and improves etc., within all should still belonging to patent covering scope of the present invention.
Claims (6)
1. the clear scar method of the movement of crystallization of adipic acid device, is characterized in that: establishing crystallizer has M crystallisation chamber, and rear N chamber of whole crystallizer produces crystallization, wherein M >=N, and front M-N dissolves clear scar in a chamber, the detailed process of clear scar is: before clear scar starts, the pressure of each crystallisation chamber is P0, be N the pressure that chamber crystallization is corresponding, the T0 moment starts mobile clear scar, at the uniform velocity rise to P1 by pressure-regulating valve by P0 in Δ T time internal pressure, the now material balance temperature rise of crystallization chamber, then pressure P 1 keeps a period of time, the indoor solution of part reaches undersaturated condition, brilliant scar is dissolved gradually, after brilliant scar has been dissolved, the T1 moment starts to recover to initial operation, initial operation is the crystallization of N chamber, in Δ T time internal pressure by P1 uniform descent to P0, the T0+ Δ T moment, clear scar finished.
2. the clear scar method of the movement of crystallization of adipic acid device according to claim 1, is characterized in that: Δ T span is set between 10-30min conventionally.
3. the clear scar method of the movement of crystallization of adipic acid device according to claim 1, is characterized in that: P0 and P1 span are set between 5mmHgA-400mmHgA.
4. the clear scar method of the movement of crystallization of adipic acid device according to claim 1, is characterized in that: each crystallisation chamber has different separately P0 and P1 setting value.
5. the clear scar method of the movement of crystallization of adipic acid device according to claim 1, is characterized in that: each crystallisation chamber rate of pressure change difference, the time having changed is identical.
6. the clear scar method of the movement of crystallization of adipic acid device according to claim 1, is characterized in that: crystallizer is also provided with flushing line.
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| CN201410347012.1A CN104107818B (en) | 2014-07-18 | 2014-07-18 | A kind of clear scar method of movement of crystallization of adipic acid device |
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| CN201410347012.1A CN104107818B (en) | 2014-07-18 | 2014-07-18 | A kind of clear scar method of movement of crystallization of adipic acid device |
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| CN104107818B CN104107818B (en) | 2016-03-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112516618A (en) * | 2020-12-17 | 2021-03-19 | 重庆华峰化工有限公司 | Adipic acid crystallization system and online scar cleaning method thereof |
Citations (8)
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|---|---|---|---|---|
| US3680621A (en) * | 1968-03-04 | 1972-08-01 | Fives Lille Cail | Crystallization installation with control system |
| JPS5452676A (en) * | 1977-10-04 | 1979-04-25 | Kobe Steel Ltd | Separating method for substances with crystallization by adiabatic pressurization |
| JPS5452678A (en) * | 1977-10-04 | 1979-04-25 | Kobe Steel Ltd | Separating method for substances utilizing high pressure |
| JP2001047062A (en) * | 1999-08-09 | 2001-02-20 | Kurita Water Ind Ltd | Treatment of leachate from landfill site |
| CN2922986Y (en) * | 2005-12-05 | 2007-07-18 | 中国石油天然气股份有限公司 | Crystallizer suitable for producing adipic acid device |
| CN202289546U (en) * | 2011-10-26 | 2012-07-04 | 化学工业第二设计院宁波工程有限公司 | Adipic acid crystallization device |
| CN102631793A (en) * | 2012-03-05 | 2012-08-15 | 郑加福 | Automatically cleaned multiple-effect evaporation crystallizer |
| CN103120861A (en) * | 2012-12-29 | 2013-05-29 | 天津听海科技有限公司 | Hexane diacid crystallization device |
-
2014
- 2014-07-18 CN CN201410347012.1A patent/CN104107818B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3680621A (en) * | 1968-03-04 | 1972-08-01 | Fives Lille Cail | Crystallization installation with control system |
| JPS5452676A (en) * | 1977-10-04 | 1979-04-25 | Kobe Steel Ltd | Separating method for substances with crystallization by adiabatic pressurization |
| JPS5452678A (en) * | 1977-10-04 | 1979-04-25 | Kobe Steel Ltd | Separating method for substances utilizing high pressure |
| JP2001047062A (en) * | 1999-08-09 | 2001-02-20 | Kurita Water Ind Ltd | Treatment of leachate from landfill site |
| CN2922986Y (en) * | 2005-12-05 | 2007-07-18 | 中国石油天然气股份有限公司 | Crystallizer suitable for producing adipic acid device |
| CN202289546U (en) * | 2011-10-26 | 2012-07-04 | 化学工业第二设计院宁波工程有限公司 | Adipic acid crystallization device |
| CN102631793A (en) * | 2012-03-05 | 2012-08-15 | 郑加福 | Automatically cleaned multiple-effect evaporation crystallizer |
| CN103120861A (en) * | 2012-12-29 | 2013-05-29 | 天津听海科技有限公司 | Hexane diacid crystallization device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112516618A (en) * | 2020-12-17 | 2021-03-19 | 重庆华峰化工有限公司 | Adipic acid crystallization system and online scar cleaning method thereof |
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| CN104107818B (en) | 2016-03-09 |
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