CN105061344B - A kind of melamine slow cooling crystallizes production method - Google Patents
A kind of melamine slow cooling crystallizes production method Download PDFInfo
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- CN105061344B CN105061344B CN201510480731.5A CN201510480731A CN105061344B CN 105061344 B CN105061344 B CN 105061344B CN 201510480731 A CN201510480731 A CN 201510480731A CN 105061344 B CN105061344 B CN 105061344B
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- melamine
- slow cooling
- gas
- heat exchanger
- shell
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/62—Purification of melamine
Abstract
Production method is crystallized the invention discloses a kind of melamine slow cooling, a slow cooling crystallizer is set after hot gas cooling, filtering and impurity removing in reaction gas, the slow cooling crystallizer includes a cylindrical housing, the many heat exchanger tubes built with conductive fluid are longitudinally provided with the shell, the upper end of the heat exchanger tube is fixed on tube sheet, lower end is connected with bar-mat reinforcement, and bar-mat reinforcement is connected by connecting shaft by the export mouth on shell with outside vibrator.Finished first using heat exchanger tube with vibrator in slow cooling crystallizer and closed, heat exchanger tube is set not only have heat exchange function, also clear up the function of heat exchange surface, and the crystallization processes process of melamine shortens, the urea washes process for consuming a large amount of power, the cooling air circulation system containing Cool gas blower are eliminated, production cost has been saved.
Description
Technical field
The invention belongs to chemical production technical field, more particularly to a kind of production method of melamine.
Background technology
At present, the dry technology for production of melamine have gas phase quenching process, the solid phase quenching crystallisation in discussion.
Gas phase quenching crystallization technological process be：Fusing urea is through being atomized and entering in reactor, in certain pressure, temperature
Under catalyst action, reaction generation melamine, ammonia, carbon dioxide gas mixture and a small amount of accessory substance.Reacted gas
Into the cooling of hot gas cooler, separate out the high boiling point by-products produced Miller amine of reaction, close white amine crystallization, the silica white in gas
End, by product are filtered out through hot-air filter.The dustless gas come out from filter is entered in crystallizer by top, with entering from middle part
150 DEG C of cold process cycles gas mixing, the quenchings entered, temperature drop is to 210 DEG C, and melamine powder crystallization is separated out, and with mixing
Gas is together from bottom discharge, and subsequently into finished product trap, melamine gathers trap bottom, by scraper and pressure spiral shell
Separator is sent out in rotation, is cooled down through fan stream and is delivered to finished product bin, finished product is packaged to produce melamine product.
The urea of melamine is not generated containing micro triamine dust and in gas at the top of the triamine trap out
And intermediate product, steamed into the water heat exchange by-product 0.15Mpa water in liquid the urine scrubbing tower, with its cooler for thering is liquid urea to circulate
Vapour, three tunnels of gas point after washing, purifying and cooling are urinated by liquid and are sent out：The first via boosted through Carrier Gas Compressor after as reaction bed
Carrier gas is recycled, and device is decrystallized as the recycling of quenching gas in the second tunnel after being boosted through Cool gas blower, the 3rd tunnel is entered at tail gas
Reason system.
There is problems with production：One is that air conditioning quantity is usually 4 times of load volume, and the preparation of a large amount of cold air need to be consumed greatly
The power of amount, has a strong impact on the power consumption of product；Two be that Cool gas blower works under the conditions of 150 DEG C or so, containing a large amount of in tail gas
Ammonia, carbon dioxide, and carry secretly a small amount of urea and with the appendicular residual of metal, enter crystallizer when pollution crystallization production
Product；Three be to react air cooling and the process of crystallization to decline reaction gas recuperation of heat amount and recuperation of heat grade, causes energy dissipation.
Solid phase quenching crystallisation technique is the deficiency for original technique, develops recirculating fluidized bed solid-phase crystallization method trimerization
Cyanamide production Technology, ciculation fluidized technology is introduced into preparation technology of melamine.In the modified technique, from reactor
The mixtures such as melamine, ammonia, carbon dioxide out are cooled to 350'C or so, into filter remove catalyst powder and
Accessory substance crystal, the melamine particles for entering back into recirculating fluidized bed crystallizer with 180 DEG C or so are mixed, 350 DEG C or so of gas
Body is cooled to 210 DEG C or so, and the melamine crystallization in gas phase is separated out, and the sensible heat of crystallization heat and partial reaction gas is then in fluidisation
Removed, used for device other parts with 1.0~1.2MPa vapor form in bed crystallizer.Isolate the gas after melamine
After body boosts through compressor：A part of Returning reactor makees carrier gas, is partly into exhaust gas recovery system.
The technique has its to shorten flow, reduces the theory of investment, but when melamine is crystallized, blocking pipeline, equipment
Problem is not solved fundamentally, production is continued on, and is used as 180 DEG C or so of melamine of cooling medium
The preparation process such as grain cooling, conveying can waste many electric power, and solid particle sensible heat is not easy to reclaim, and it is remaining that melamine reacts
Heat can cause very big waste, therefore the technology never has industrialization.
The content of the invention
Melamine is white monocrystalline or white powder, 300 DEG C of sublimation temperature, and pure melamine gas is sublimated the knot of precipitation
Crystalline flour end is fluffy, easily cleaning.
The present invention is to cool to complete the crystallization process of sublimating of melamine in reaction gas by heat exchanger indirect type, is realized
The recovery profit Rong of reaction gas used heat, reaches energy-saving purpose.
The purpose of the present invention is achieved through the following technical solutions：After hot gas cooling, filtering and impurity removing in reaction gas
One slow cooling crystallizer is set, and the slow cooling crystallizer includes a cylindrical housing, and shell upper is provided with steam (vapor) outlet, outer casing underpart
Provided with crystallization gas, powder outlet, the upper lateral part of shell, which is additionally provided with purified gas entrance and desalination water out, the shell, to be longitudinally provided with
The many heat exchanger tubes built with conductive fluid, the upper end of the heat exchanger tube is fixed on tube sheet, and lower end is connected with bar-mat reinforcement, bar-mat reinforcement
It is connected by connecting shaft by the export mouth on shell with outside vibrator, provided with sealing between the connecting shaft and export mouth
Pad.Conductive fluid is in bottom high-temperature region by thermal evaporation in heat exchanger tube during work, and the gas of gasification exchanges heat on heat exchanger tube top and water to be produced
Gas is back to heat exchange bottom of the tube while condensing and becoming liquid in producing water vapor, pipe, and so on circulates.
When melamine crystallization is attached to heat exchange pipe surface, the vibrations of vibrator are delivered to bar-mat reinforcement by connecting shaft,
Heat exchanger tube vibrations are driven, melamine is come off, persistently keeps its heat exchange function.
Go out the generation gas of reactor through being cooled to 350 DEG C, be filtered to remove impurity, dust-free purification gas enters slow cooling by top
Crystallizer, reaction gas is cooled to 210 DEG C by heat exchanger tube in slow cooling crystallizer, and melamine is sublimated, separated out, and crystallization process is put
The heat gone out is by Water Sproading, 1.0~1.2MPa of by-product middle pressure steam.
Melamine powder crystallization is separated through trap, is entered compressor and is pressurised into reaction system offer carrier gas, redundance
Tail gas remove exhaust gas recovery system.
With the difference of prior art
1st, the crystallization processes process of melamine shortens, and eliminates and consumes the urea washes process of a large amount of power, containing cold air
The cooling air circulation system of blower fan.
2nd, finished first using heat exchanger tube and vibrator in slow cooling crystallizer and closed, heat exchanger tube is not only had heat exchange function, also
There is the function of cleaning heat exchange surface.
Beneficial effects of the present invention：
1st, by setting slow cooling crystallizer, gas used heat of the reaction gas at 350 DEG C -210 DEG C is made（Particularly melamine
234 kcal/kg crystallization heat）, reclaimed, reclaimed compared with gas phase quenching technique in the form of 1-1.2Mpa medium pressure steams
0.15Mpa water vapours compare, the value of recuperation of heat is greatly improved.
2nd, Cool gas blower, urine are eliminated and washes the cold air Preparation equipment such as tower, power consumption significantly declines.
3rd, civilwork engineering quantity declines, and floor space is small, and the investment of device can be made significantly to decline.
Brief description of the drawings
The embodiment that the invention will now be described in detail with reference to the accompanying drawings
Fig. 1 is slow cooling crystallizer sectional view of the invention
Fig. 2 is process chart of the invention
Fig. 3 is the technique flow graph of prior art
In figure：1st, shell 2, steam (vapor) outlet 3, crystallization gas, powder export 4, purified gas entrance 5, desalination water out 6, led
Hydrothermal solution 7, heat exchanger tube 8, tube sheet 9, bar-mat reinforcement 10, connecting shaft 11, vibrator 12, sealing gasket.
Embodiment
As shown in Figure 1, 2, fusing urea enters in reactor after atomization generates gaseous melamine, and with ammonia and dioxy
Carrier gas based on change carbon mixed gas together, obtains reacting purified gas through heat exchange cooling, filtering and impurity removing.The gas is entered by top
Slow cooling crystallizer, slow cooling crystallizer includes a cylindrical housing 1, and the top of shell 12 is provided with steam (vapor) outlet, and the bottom of shell 1 is provided with knot
Brilliant gas, powder outlet 3, the upper lateral part of shell 1, which is additionally provided with purified gas entrance 4 and desalination water out 5, shell 1, is longitudinally provided with many
Built with the heat exchanger tube 7 of conductive fluid 6, the upper end of heat exchanger tube 7 is fixed on tube sheet 8, and lower end is connected with bar-mat reinforcement 9, bar-mat reinforcement 9 by
Connecting shaft 10 is connected by the export mouth on shell 1 with outside vibrator 11, provided with close between connecting shaft 10 and export mouth
Packing 12.Reaction gas is cooled to less than 210 DEG C by the heat exchanger tube in device in slow cooling crystallizer, and melamine sublimates, separates out powder
End crystallization, cooling, bottom conductive fluid of the heat in heat exchanger tube of crystallization process are reclaimed and are vaporized, and conductive fluid steam is being changed
Heat pipe top produces 1-1.2MPa water vapours with water heat exchange.
After device puts into production, the crystallization of powdery melamine is liable to stick on the surface of heat exchanger tube 7, influences changing for crystallizer
The thermal efficiency, at this moment starts vibrator 11, and the vibrations of vibrator 11 are delivered to bar-mat reinforcement 9 by connecting shaft 10, drive heat exchanger tube shake
It is dynamic, the melamine powder for being attached to heat exchange pipe surface is come off, persistently keep its heat exchange function.
The melamine powder separated out is crystallized, is entered with gas in trap, melamine production is obtained through separation and recovery
Product.Purified gas, it is most of to enter Carrier Gas Compressor entrance, reactor inlet pressure is boosted to after compression, as anti-
Device carrier gas source of the gas is answered, remainder is directly discharged into exhaust gas recovery system, for preparing liquefied ammonia, ammoniacal liquor and other ammonolysis products.
Claims (2)
1. a kind of melamine slow cooling crystallizes production method, a slow cooling is set after the hot gas cooling, filtering and impurity removing in reaction gas
Crystallizer, the slow cooling crystallizer includes a cylindrical housing, and shell upper is provided with steam (vapor) outlet, and outer casing underpart is provided with crystallization
Gas, powder outlet, the upper lateral part of shell are additionally provided with purified gas entrance and desalination water out, it is characterised in that longitudinally set in the shell
There are many heat exchanger tubes built with conductive fluid, the upper end of the heat exchanger tube is fixed on tube sheet, and lower end is connected with bar-mat reinforcement, reinforcing bar
Net is connected by connecting shaft by the export mouth on shell with outside vibrator.
2. a kind of melamine slow cooling crystallization production method as claimed in claim 1, it is characterised in that the connecting shaft is with leading
Sealing gasket is provided between outlet.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510480731.5A CN105061344B (en) | 2015-08-09 | 2015-08-09 | A kind of melamine slow cooling crystallizes production method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510480731.5A CN105061344B (en) | 2015-08-09 | 2015-08-09 | A kind of melamine slow cooling crystallizes production method |
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| Publication Number | Publication Date |
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| CN105061344A CN105061344A (en) | 2015-11-18 |
| CN105061344B true CN105061344B (en) | 2017-09-22 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558783A (en) * | 2018-06-08 | 2018-09-21 | 程克信 | A kind of melamine complete alternation production technology and device |
| CN109529397A (en) * | 2018-12-28 | 2019-03-29 | 四川金象赛瑞化工股份有限公司 | One kind is sublimated crystallizer and method for crystallising |
| CN112090105B (en) * | 2020-09-11 | 2021-06-22 | 山东博苑医药化学股份有限公司 | Method for refining iodine by circulating air sublimation |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276544A (en) * | 2011-05-08 | 2011-12-14 | 徐建华 | Production equipment, energy-saving production system and production method for melamine |
| WO2012146056A1 (en) * | 2011-04-28 | 2012-11-01 | 四川金象赛瑞化工股份有限公司 | Energy-saving low-cost system and process for producing melamine by means of gas quenching |
| CN103102320A (en) * | 2013-01-17 | 2013-05-15 | 李鑫 | Production method of melamine by slow cooling crystallization |
| CN204084299U (en) * | 2014-09-08 | 2015-01-07 | 山东省舜天化工集团有限公司 | Residual heat using device in a kind of preparation technology of melamine |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202128942U (en) * | 2010-12-23 | 2012-02-01 | 山东三和化工有限公司 | Melamine cooling collector |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012146056A1 (en) * | 2011-04-28 | 2012-11-01 | 四川金象赛瑞化工股份有限公司 | Energy-saving low-cost system and process for producing melamine by means of gas quenching |
| CN102276544A (en) * | 2011-05-08 | 2011-12-14 | 徐建华 | Production equipment, energy-saving production system and production method for melamine |
| CN202107649U (en) * | 2011-05-08 | 2012-01-11 | 徐建华 | Production device for melamine and energy-saving production system |
| CN103102320A (en) * | 2013-01-17 | 2013-05-15 | 李鑫 | Production method of melamine by slow cooling crystallization |
| CN204084299U (en) * | 2014-09-08 | 2015-01-07 | 山东省舜天化工集团有限公司 | Residual heat using device in a kind of preparation technology of melamine |
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| CN105061344A (en) | 2015-11-18 |
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