CN106430240B - A kind of ammonium hydroxide continuous process system - Google Patents
A kind of ammonium hydroxide continuous process system Download PDFInfo
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- CN106430240B CN106430240B CN201610840532.5A CN201610840532A CN106430240B CN 106430240 B CN106430240 B CN 106430240B CN 201610840532 A CN201610840532 A CN 201610840532A CN 106430240 B CN106430240 B CN 106430240B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/022—Preparation of aqueous ammonia solutions, i.e. ammonia water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/024—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Gas Separation By Absorption (AREA)
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Abstract
The present invention relates to a kind of ammonium hydroxide continuous process systems, including liquid ammonia material storage tank, prewashing tower, two-stage scrubbing tower, two-stage absorption tower, heat exchanger and the tail gas absorber and cooling-water machine sequentially arranged；Configured with two absorption slots below two-stage absorption tower, achievable synchronization or alternately operating are closed or opened by valve on connecting line by the piping connection with valve, the first absorption slot and the second absorption slot with two-stage scrubbing tower respectively；Two absorb the reconfiguration of slot discharge port and have circulating pump and discharge pump, the import of circulating pump to absorb slot with two respectively by the pipeline with valve and connect, and the outlet of circulating pump is connect by the pipeline with valve with heat exchanger and finished pot；The import of discharge pump and discharge pump absorbs slot with two respectively by the pipeline with valve and connect, and the replacement operation of cost pump and circulating pump can be achieved by the opening and closing of valve.The present invention has the advantages that simple production process, production security are good, product purity is high, conversion ratio is high, production cost is low.
Description
Technical field
The invention belongs to ammonium hydroxide production systems, and in particular to a kind of energy saving, continuous ammonium hydroxide production system.
Background technology
Ammonium hydroxide is widely used in the fields such as agricultural, industry, military affairs, and domestic ammonium hydroxide Preparation equipment is all divided into industry at present
Ammonium hydroxide, electron level ammonium hydroxide, SILVER REAGENT ammonium hydroxide preparation facilities, aforementioned device have a single function when in use, cannot use a kind of equipment
The ammonium hydroxide of various grades is prepared, and most equipment can only prepare technical grade ammonium hydroxide, and ultra-clean high-purity ammonium hydroxide cannot be prepared.
The application for a patent for invention of publication No. CN105293523A discloses a kind of ketazine process hydrazine hydrate production raw material ammonia water
Continuous preparation method, by liquid ammonia gasification and absorb and two level absorb continuously prepare concentration stabilization ammonium hydroxide for ketone connect
Nitrogen method hydrazine hydrate production system uses.By using densitometer on-line checking, collaboration liquid ammonia gasification amount, vapor pressure automatically control
The density of ammonium hydroxide obtains accurate and stable control in fixed value, ammonium hydroxide content.Utilize liquid ammonia gasification heat absorption, gas ammonia exothermic dissolution
Principle complete ammonium hydroxide cold and hot exchange required when producing, provide heat and cold without extraneous, it is energy-saving.By excessive
Soft water is absorbed with a small amount of ammonia, is completed the whole of ammonia and is absorbed, exhaust emissions is up to standard, absorbs the weak aqua ammonia conduct of ammonia
The absorbent of first order absorption is generated without waste water, waste liquid in entire production process.
However, existing ammonium hydroxide preparation system be widely present production slowly, the low defect of efficiency, especially for producing
The accurate ammonium hydroxide of purity higher, concentration.
Invention content
The technical problem to be solved by the present invention is to provide a kind of ammonium hydroxide continuous process system for the above-mentioned prior art, carry
High product purities, ammonia conversion capability, realization are worked continuously, and production efficiency and system energy efficiency are improved.
Technical solution is used by the present invention solves the above problems：A kind of ammonium hydroxide continuous process system, including sequentially cloth
Liquid ammonia material storage tank, prewashing tower, two-stage scrubbing tower, two-stage absorption tower, heat exchanger and the tail gas absorber and cooling-water machine set, it is described
Two-stage scrubbing tower is separately configured with washing pump, and the washing pump is connected by circulation line with corresponding scrubbing tower and realized
Cycle in scrubbing tower；Configured with two absorption slots below the two-stage absorption tower：First absorb slot respectively with two-stage absorption tower
By the piping connection with valve, second absorbs slot is absorbed with two-stage absorption tower by the piping connection with valve, first respectively
Slot and the second absorption slot close or open achievable synchronization or alternately operating by valve on connecting line, and two absorb slots difference
With pure water water inlet；Described two absorb slot discharge port and are further configured with circulating pump and discharge pump, the circulating pump
Import absorbs slots with two respectively by the pipeline with valve and connect, the outlet of the circulating pump by the pipeline with valve with change
Hot device connection, is taken away the heat discharged in absorption process through heat exchanger with realizing；The import of the discharge pump passes through band valve
Pipeline absorb slots with two respectively and connect, the outlet of the discharge pump by the pipeline take over finished pot with valve, using
Filtering packing obtains ammonium hydroxide finished product, and the export pipeline of the circulating pump is provided with the branch with valve, is connected to finished pot；It is described at
The export pipeline of product pump is provided with the branch with valve, is connected to heat exchanger, and the circulating pump can be substituted for each other work with discharge pump
Industry or alternately operating；The heat exchanger is concatenated two-stage heat exchanger, and the outlet of the two-stage heat exchanger is in parallel and passes through pipeline
Docking two-stage absorption tower respectively；The offgas outlet on the second level absorption tower in the two-stage absorption tower docks tail gas absorber, institute
It states and is configured with tail gas absorption groove below tail gas absorber, the tail gas absorption groove discharge port connects tail washings circulating pump, which follows
Ring pump connects the cyclic absorption that tail gas absorber realizes tail gas by circulation line；Two below two-stage absorption tower absorb slots and
Two-stage heat exchanger and tail gas absorption groove are separately connected the cooling water inlet pipe and cooling water return pipe of cooling-water machine.
Preferable setting is the prewashing tower, two-stage scrubbing tower, two-stage absorption tower, two absorption slots, tail gas absorption grooves point
It is not provided with liquid level gauge, being smoothed out for production is realized in personnel on site's monitoring easy to operation.
Based on the production technology of above-mentioned ammonium hydroxide continuous process system, the liquefied ammonia in liquid ammonia material storage tank enters prewashing tower,
The ammonia that gasification obtains in prewashing tower is passed through first order scrubbing tower and obtains more pure ammonia through level-one washing, is washed from the first order
It washs the pure ammonia that tower comes out to enter second level scrubbing tower and gone the net absorbing pure water of superelevation at ammonium hydroxide, and it is higher to release purity
Ammonia, prewashing and two-stage washing mainly remove metal and nonmetallic inclusion in ammonia.
Ammonia after washing enters first order absorption tower after gas-liquid separation, by the net pure water cycle spray of superelevation in absorption tower
Leaching absorbs, and the remaining ultra-clean ammonia of absorption, which enters back into the absorption tower of the second level, in first order absorption tower continues cycling through spray-absorption,
The tail gas that two level absorption generates is discharged into tail gas absorber and continues cycling through spray-absorption, until tail gas is emission-free by all absorption realizations
Discharge；The heat that absorption process generates is taken away by heat exchanger, and heat transferring medium uses cooling water；Two below two-stage absorption tower
It absorbs slot and alternately operating is realized by the opening and closing of respective valves, keep production continuously uninterrupted, the ammonium hydroxide absorbed in slot closes after testing
Finished pot is squeezed into through discharge pump after lattice, packing is filtered and obtains ultra-pure ammonium hydroxide finished product.
Preferably, two ammonium hydroxide absorbed in slot are pumped into heat exchanger through circulating pump, and the ammonium hydroxide after heat exchange is back to respectively again
Circulated sprinkling absorption is carried out in two-stage absorption tower；Two absorb ammonium hydroxide qualified after testing in slot and are pumped into finished pot through discharge pump；
The replacement operation of circulating pump and discharge pump can be achieved by the opening and closing of respective valves.
Compared with the prior art, the advantages of the present invention are as follows：The ammonium hydroxide continuous process system of the present invention is cut using valve
The uninterrupted production of realization is brought, by the way that two absorption slots are arranged, complete to absorb when any of which absorbs slot, closes liquid flowing valve,
Bottom valve is opened, racking room is delivered to by discharge pump, during this, in order to not influence continuous production, it is ensured that the production product of ammonium hydroxide
Matter opens simultaneously another absorption slot, continues the constant absorption of ammonium hydroxide, and this continuous small lot absorbs the ammonium hydroxide producer of operation
Formula can also stablize the concentration and finished product output capacity of ammonium hydroxide, it is ensured that the stabilization and production security of product quality.
In addition, two absorb slots configuration circulating pumps and discharge pump by the opening and closing of valve on pipeline, it can be achieved that beating cycle
It with the switching of two kinds of functions of the product that break into, also ensures that continuous production is uninterrupted, helps to improve production efficiency, reduce redundant equipment
Energy consumption.
Ammonium hydroxide continuous producing method of the present invention have simple production process, production security is good, product purity is high, conversion ratio
Advantage high, production cost is low.
Description of the drawings
Fig. 1 is the structural schematic diagram of ammonium hydroxide continuous process system in the embodiment of the present invention.
Specific implementation mode
Below in conjunction with attached drawing embodiment, present invention is further described in detail.
As shown in Figure 1, the ammonium hydroxide continuous process system in the present embodiment, including the liquid ammonia material storage tank 1, pre- sequentially arranged
Wash tower 2, two-stage scrubbing tower 3, two-stage absorption tower 5,6, heat exchanger 11 and tail gas absorber 12 and cooling-water machine 15, two-stage scrubbing tower with
Two-stage is provided with gas-liquid separation filter between absorption tower.Two-stage scrubbing tower 3 is separately configured with washing pump 4, described to wash
It washs pump 4 and connects the cycle operation for realizing material in scrubbing tower 3 by circulation line with corresponding scrubbing tower 3.
One absorption slot of each configuration in 5,6 lower section of two-stage absorption tower：First absorbs slot 7 passes through band valve with two-stage absorption tower respectively
The piping connection of door, second absorbs slot 8 respectively with two-stage absorption tower by the piping connection with valve, i.e., two absorption slots are mutual
Independent, first absorbs the achievable synchronous or alternately operating of opening and closing that slot 7 absorbs slot 8 by valve on connecting line with second,
The ammonium hydroxide product in the absorption slot can be pumped into finished pot after detecting the ammonium hydroxide qualification in any absorption slot, opened simultaneously
Another absorption slot takes over work, it is ensured that and production is continuous uninterrupted, meanwhile, the mode that this continuous small lot absorbs operation also can
Enough stablize the concentration and finished product output capacity of ammonium hydroxide.In addition, two absorption slots are respectively provided with pure water water inlet.
Two absorb 7,8 discharge port of slot and are further configured with circulating pump 9 and discharge pump 10, and the import of circulating pump 9 passes through
Pipeline with valve absorbs slot with two respectively and connect, and the outlet of circulating pump 9 is connect by the pipeline with valve with heat exchanger 11,
The heat discharged in absorption process is taken away through heat exchanger with realizing.The import of discharge pump 10 by the pipeline with valve respectively with
Two absorb slot connection, and the outlet of the discharge pump 10 passes through the pipeline take over finished pot with valve（It is not shown in figure）, then pass through
Filtering packing obtains ammonium hydroxide finished product.The export pipeline of circulating pump 9 is provided with the branch with valve, then is connected to finished pot；Finished product
The export pipeline of pump 10 is provided with the branch with valve, then is connected to heat exchanger 11, makes circulating pump 9 and finished product by the opening and closing of valve
Pump 10 can be substituted for each other operation or alternately operating.
The present embodiment heat exchanger is concatenated two-stage heat exchanger, and the outlet of two-stage heat exchanger is separately right by pipeline
Connect two-stage absorption tower 5,6.
The offgas outlet on the second level absorption tower 6 in above-mentioned two-stage absorption tower 5,6 docks tail gas absorber 12, tail gas absorption
12 lower section of tower is configured with tail gas absorption groove 13, and 13 discharge port of tail gas absorption groove connects tail washings circulating pump 14, the tail washings circulating pump 14
The realization of tail gas absorber 12 is connected to the cyclic absorption of tail gas, the emission-free discharge of system by circulation line.
Two absorption slots 7,8 and two-stage heat exchanger 11 and tail gas absorption groove 13 below two-stage absorption tower are separately connected cold water
The cooling water inlet pipe and cooling water return pipe of machine 15.
Further, prewashing tower 2, two-stage scrubbing tower 3,5,6, two, two-stage absorption tower absorb slot 7,8, tail gas absorber
12, tail gas absorption groove 13 is respectively arranged with liquid level gauge.
Production technology based on above-mentioned ammonium hydroxide continuous process system：Liquefied ammonia in liquid ammonia material storage tank enters prewashing tower,
The ammonia that gasification obtains in prewashing tower is passed through first order scrubbing tower and obtains more pure ammonia through level-one washing absorption, from first
The pure ammonia that grade scrubbing tower comes out enters second level scrubbing tower and is gone the net absorbing pure water of superelevation at ammonium hydroxide, and releases purity more
High ammonia, prewashing and two-stage washing mainly remove metal in ammonia and obtain high-purity ammonia with nonmetallic inclusion.
Ammonia after washing enters first order absorption tower after gas-liquid separation, by the net pure water cycle spray of superelevation in absorption tower
Leaching absorbs, and the remaining ultra-clean ammonia of absorption, which enters in the absorption tower of the second level, in first order absorption tower continues cycling through spray-absorption, and two
The tail gas that grade absorption generates is discharged into tail gas absorber and continues cycling through spray-absorption, until tail gas is all absorbed the emission-free row of realization
It puts.The heat that absorption process generates is taken away by heat exchanger, and heat transferring medium uses cooling water.Two suctions below two-stage absorption tower
It receives slot and alternately operating is realized by the opening and closing of respective valves, keep production continuously uninterrupted, the ammonium hydroxide absorbed in slot is qualified after testing
Finished pot is squeezed by discharge pump, packing is filtered and obtains ultra-pure ammonium hydroxide finished product.
Two ammonium hydroxide absorbed in slot are pumped into heat exchanger through circulating pump, and the ammonium hydroxide after heat exchange is back to two-stage absorption respectively again
Circulated sprinkling absorption is carried out in tower；Two absorb ammonium hydroxide qualified after testing in slot and are pumped into finished pot through discharge pump；By corresponding
The replacement operation of circulating pump and discharge pump can be achieved in the opening and closing of valve.
The setting of system process parameters：
Technological parameter is the central factor for influencing product quality, in process of manufacture, the confirmation and choosing of technological parameter
Select be control and stabilized product quality basic solution.In the present embodiment, the target output of ultra-clean high-purity ammonium hydroxide is 30% ammonia
Water 6 tons/24 hours, specific process parameter is as follows：
1. the charging setting of liquid ammonia material steel cylinder：
Whether the conversion that the charging rate of liquid ammonia material is related to the material balance of whole system, raw material and finished product is reasonable.
If charging is too fast, then insufficient for ammonia absorption, a large amount of tail gas enter tail gas absorption tank, if excessively slow, then cause system
Working time is long, is unfavorable for completing throughput requirements.When starting charging, liquid ammonia steel bottle valve is slowly opened, until airline pressure
Table shows 0.7Mpa.
2. prewashing tower water level settings：
It is placed in advance in ultra-clean pure water, can be worked as a buffer, liquefied ammonia meets water heat release, so that it is vaporized bubbling and can filter
Fall metal or nonmetallic inclusion in technical grade liquefied ammonia and obtains pre- washed ammonia.Prewashing tower height:1500mm, diameter:
400mm is placed in advance in ultra-clean pure water to the scale of liquid level gauge water level 800mm.
3. scrubbing tower water level settings:
Pre- washed ammonia enters two-stage scrubbing tower and carries out cycle washing, and the double-deck filler can filter out most of impurity, wash
Wash tower height：3500mm, diameter:400mm is placed in advance in ultra-clean pure water to the scale of liquid level gauge water level 670mm.
4. absorbing slot water level settings：
Systemic presupposition set the goal yield be 2 ton days, a concentration of 30%, this subsystem use 3500L volumes absorption slot, adopt
It is designed with chuck, recirculated cooling water is flowed into chuck, takes away the heat released in absorption process.It is first placed in advance in absorption slot super
Net pure water 1400L opens circulating pump and carries out cyclic absorption ammonia, until absorbing ammonium hydroxide in slot reaches aimed concn.
5. cooling-water machine cooling water temperature is set：
Absorbing pure water ammonia is at the process that ammonium hydroxide is a very exothermic, and the solubility of ammonia in water is with temperature liter
High and reduces, during cyclic absorption, we take away heat with heat exchanger, using vertical pipe type progress heat friendship in heat exchanger
It changes, cooling water is prepared by the cooling-water machine of 11KW in standpipe, and temperature is 15 DEG C.
6. absorption tower, scrubbing tower packed height：
Firstly, since the gap between filler and tower wall is big compared with the gap among packing layer, therefore liquid is easy to tower wall
It flows and influences mass transfer effect, commonly referred to as this is wall effect.For high tower, wall effect is even more serious, therefore, commonly uses
Segmentation loads or gets up to solve the problems, such as this with liquid redistribution.Under normal circumstances, height H and the filler tower diameter of filler filling it
Than being more suitable for 2~6, it can effectively evade wall effect.Our this secondary design tower height：3500mm, diameter：400mm, filler
Height takes 2D i.e. 800mm, and it is 400mm to be divided to two sections of fillings, every section of packed height.
Secondly, the sequence of filler is also required, system design takes out of order filler, allow cycle in view of increasing stroke
Pure water fully absorb ammonia and can preferably play the role of filtering out residual impurity.
In addition to the implementation, all to use equivalent transformation or equivalent replacement the invention also includes there is an other embodiment
The technical solution that mode is formed should all be fallen within the scope of the hereto appended claims.
Claims (2)
1. a kind of ammonium hydroxide continuous production processes, it is characterised in that：Its system includes the liquid ammonia material storage tank sequentially arranged, prewashing
Tower, two-stage scrubbing tower, two-stage absorption tower, heat exchanger and tail gas absorber and cooling-water machine, the two-stage scrubbing tower is separately
Configured with washing pump, the washing pump connects the cycle realized in scrubbing tower with corresponding scrubbing tower by circulation line；
Configured with two absorption slots below the two-stage absorption tower：First absorption slot passes through with two-stage absorption tower with valve respectively
Piping connection, second absorbs slot respectively with two-stage absorption tower by the piping connection with valve, and first, which absorbs slot and second, absorbs
Slot closes or opens achievable synchronization or alternately operating by valve on connecting line, and two absorption slots are respectively provided with pure water water inlet
Mouthful；
Described two absorb slot discharge port and are further configured with circulating pump and discharge pump, and the import of the circulating pump passes through band valve
The pipeline of door absorbs slot with two respectively and connect, and the outlet of the circulating pump is connect by the pipeline with valve with heat exchanger, with
Realization takes away the heat discharged in absorption process through heat exchanger；The import of the discharge pump by the pipeline with valve respectively with
Two absorb slot connection, and the outlet of the discharge pump is obtained by the pipeline take over finished pot with valve using filtering packing
The export pipeline of ammonium hydroxide finished product, the circulating pump is provided with the branch with valve, is connected to finished pot；The outlet of the discharge pump
Road is provided with the branch with valve, is connected to heat exchanger, and the circulating pump can be substituted for each other operation or alternately operating with discharge pump；
The heat exchanger is concatenated two-stage heat exchanger, and the outlet of the two-stage heat exchanger is in parallel and docks two respectively by pipeline
Grade absorption tower；
The offgas outlet on the second level absorption tower in the two-stage absorption tower docks tail gas absorber, the tail gas absorber lower section
Configured with tail gas absorption groove, the tail gas absorption groove discharge port connects tail washings circulating pump, which passes through circulation line
Connect the cyclic absorption that tail gas absorber realizes tail gas；
Two absorption slots and two-stage heat exchanger and tail gas absorption groove below two-stage absorption tower are separately connected the cooling water of cooling-water machine
Water inlet pipe and cooling water return pipe；
The prewashing tower, two-stage scrubbing tower, two-stage absorption tower, two absorption slots, tail gas absorption grooves are respectively arranged with liquid level gauge；
Liquefied ammonia in liquid ammonia material storage tank enters prewashing tower, and the obtained ammonia that gasifies in prewashing tower is passed through first order scrubbing tower through one
Grade washing obtains more pure ammonia, and the pure ammonia come out from first order scrubbing tower enters second level scrubbing tower and gone superelevation
Net absorbing pure water releases the higher ammonia of purity at ammonium hydroxide, prewashing and two-stage washing mainly remove in ammonia metal with
Nonmetallic inclusion；
Ammonia after washing enters first order absorption tower after gas-liquid separation, is inhaled by the net pure water circulated sprinkling of superelevation in absorption tower
It receives, the remaining ultra-clean ammonia of absorption, which enters in the absorption tower of the second level, in first order absorption tower continues cycling through spray-absorption, and two level is inhaled
The tail gas that receipts generate is discharged into tail gas absorber and continues cycling through spray-absorption, until tail gas is all absorbed the emission-free discharge of realization；
The heat that absorption process generates is taken away by heat exchanger, and heat transferring medium uses cooling water；Two absorptions below two-stage absorption tower
Slot realizes alternately operating by the opening and closing of respective valves, keeps production continuously uninterrupted, and the ammonium hydroxide in absorption slot is after testing after qualification
Finished pot is squeezed into through discharge pump, packing is filtered and obtains ultra-pure ammonium hydroxide finished product.
2. according to claim 1 ammonium hydroxide continuous production processes, it is characterised in that：Two ammonium hydroxide absorbed in slot are pumped into through circulating pump
Heat exchanger, the ammonium hydroxide after heat exchange are back to progress circulated sprinkling absorption in two-stage absorption tower respectively again；Two absorb in slot through inspection
It surveys qualified ammonium hydroxide and is pumped into finished pot through discharge pump；The replacement that circulating pump and discharge pump can be achieved by the opening and closing of respective valves is made
Industry.
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| CN109455735B (en) * | 2018-12-27 | 2022-04-19 | 中核北方核燃料元件有限公司 | Chemical pure ammonia water preparation system and method |
| CN111992172B (en) * | 2020-08-03 | 2022-04-19 | 界首市南都华宇电源有限公司 | Collecting device and collecting method for ammonia water preparation |
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| CN106629773A (en) * | 2016-09-22 | 2017-05-10 | 江苏中德电子材料科技有限公司 | Energy-saving continuous ultra-clean high-purity ammonium hydroxide production system |
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| US6183720B1 (en) * | 1997-04-11 | 2001-02-06 | Air Liquide Electronics Labeille | Process and apparatus for producing high-purity chemicals for the microelectronics industry |
| CN101003361A (en) * | 2007-01-08 | 2007-07-25 | 战玉柏 | Method and equipment for preparing super clean, high purified hydrofluoric acid |
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