CN103848406A - Method for continuously separating water-based hydroxylammonium salt by use of demister - Google Patents
Method for continuously separating water-based hydroxylammonium salt by use of demister Download PDFInfo
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Abstract
The invention discloses a method for continuously preparing hydroxylammonium in a hydrogenation reactor by use of hydrogenated nitrate or nitrogen oxide to form hydroxylammonium, ammonium, nitrogen and nitrous oxide. The hydrogenation reactor comprises a) a demister, b) a gas collection area and c) a hydroxylammonium salt synthesis area, wherein the hydroxylammonium salt synthesis area comprises an aqueous phase and a gas phase. The method comprises the following steps: I) collecting the gas phase in the gas collection area; II) optionally, spraying water drops to the collected gas phase; III) passing the gas phase collected in the step I) or the collected gas phase with the water drops in the step II) through the demister [B]; and IV) recycling the liquid containing coagulated water-based liquid drops from the demister [B], wherein the water-based liquid drops contain hydroxylammonium salt, and at least one part of the liquid recycled from the demister [B] in the step IV) is added in the hydroxylammonium salt synthesis area.
Description
Technical field
The present invention relates to a kind of method that separates the hydroxyl ammonium salt that contains inorganic process liquid drop from hydrogeneous gas phase with successive processes, the method comprises passes through mist eliminator by hydrogeneous gas phase, the inorganic industrial liquid drop that wherein said gas phase contains aquosity hydroxyl ammonium salt, reclaims the liquid phase of the aquosity hydroxyl ammonium salt of separation and the liquid phase of the aquosity hydroxyl ammonium salt of at least a portion separation is drawn and got back to the synthetic district of hydroxyl ammonium salt.
Background technology
The important use of hydroxyl ammonium salt is to prepare oxime from ketone or aldehyde, particularly prepares cyclohexanone-oxime by pimelinketone.With regard to the preparation of this oxime, circulation method is known, and wherein moisture acidic buffer reaction medium synthesizes district and the maintenance circulation of the synthetic district of oxime by hydroxyl ammonium salt.Buffering salt, for example basic salt and/or ammonium salt acidic buffer that reaction medium is derived by for example phosphoric acid and/or sulfuric acid and these acid.In the synthetic district of hydroxyl ammonium salt, nitrate ion or oxynitrides in the moisture inorganic process liquid of circulation are transformed into hydroxylammonium with hydrogen.
Input fresh hydrogen is synthesized district to hydroxyl ammonium salt, and from system, regularly purifies a certain amount of gas to maintain constant hydrogen partial pressure.Purge gas comprises rare gas element composition in fresh hydrogen and the gaseous by-product nitrogen (N of generation
2) and nitrous oxide (N
2o).
Hydroxylammonium reacts with free buffering acid and forms corresponding hydroxyl ammonium salt, and by the synthetic district of this hydroxyl ammonium salt input oxime, it generates corresponding oxime with reactive ketone there, discharges sour simultaneously subsequently.Isolate oxime from reaction medium after, reaction medium is recycled to the synthetic district of hydroxyl ammonium salt and adds fresh nitrate ion or oxynitrides in reaction medium.
By phosphoric acid and the synthetic hydroxyl ammonium salt of nitrate solution in the situation that, above-mentioned chemical reaction is expressed as follows:
Reaction 1) prepare hydroxylammonium in hydroxyl ammonium salt synthesis stage:
2H
3PO
4+NO
3 -+3H
2→NH
3OH
++2H
2PO
4 -+2H
2O
Reaction 2) prepare oxime in the synthetic district of oxime:
Reaction 3) isolate the oxime of formation after, with HNO
3form supplement new nitrate ion:
H
3PO
4+H
2PO
4 -+HNO
3+3H
2O→2H
3PO
4+NO
3 -+3H
2O
First reaction is heterogeneous catalysis.Preferably, catalyzer exists as the disperse phase in liquid reaction mixture using the form of homodisperse solid.
In hydroxylammonium salt solution, the reaction mixture of the first step is the moisture inorganic process liquid containing solid catalyst particle suspensoid.
From reaction process, moisture inorganic process liquid can contain intermediate material, for example azanol or ammonia, and it also can be turned to for example hydroxylammonium or ammonium by proton.That is to say, according to the present invention, azanol and hydroxylammonium can be interpreted as azanol and/or hydroxylammonium, and ammonia and ammonium can be understood as ammonia and/or ammonium simultaneously.
Before, preferably from this moisture inorganic process liquid, isolate solid catalyst particle this moisture inorganic process liquid being input to the synthetic district of oxime (reaction 2).After filtration, this moisture inorganic process liquid is hydroxylammonium salt solution filtrate.
Such process comprises DSM's
(reference example is as H.J.Damme, J.T.van Goolen and A.H.de Rooij, Cyclohexanone oxime made without by-product (NH for process
4)
2sO
4, July10,1972, Chemical Engineering; Pp54/55or Ullmann's Encyclopedia of Industrial Chemistry (2005) at page6/7under chapter Caprolactam).
Although the preparation of hydroxylammonium is in decades known and also for many years studied, the existing still Shortcomings of the commercial run with persistence that improves known preparation method.
US20050047987 discloses a kind of method accompanying method of manufacturing hydroxylammonium salt and has comprised following steps:
A. in reaction mixture, input gaseous hydrogen, described reaction mixture comprises a kind of aqueous reaction medium and gas phase;
B. in reaction mixture, with hydrogen catalytic reduction nitride or oxynitride generation azanol;
C. gas recovery mixture from reaction mixture, the non-hydrogen component that affiliated gaseous mixture comprises gaseous hydrogen and gaseous state;
D. from gaseous mixture, be separated to the non-hydrogen component of the gaseous state of small part, obtain the gas that is rich in hydrogen; And
E. the gas that is rich in hydrogen is passed into hydrogenation zone.
Hydrogeneous gaseous mixture leaves hydrogenation zone, and this gaseous mixture contains mist, the moisture inorganic process liquid drop that described mist contains residual aquosity hydroxyl ammonium salt.Residual due to these drops, as hydroxylammonium, phosphoric acid salt and nitrate, valuable chemical composition can be lost in waste gas.This can produce negative influence to the variable cost in hydroxylammonium production process.
Preferably, be the rare gas element accumulation that prevents that similar nitrogen is such, the gaseous mixture that part is contained to hydrogen is discharged as waste gas.The gaseous mixture of other hydrogen must pressurize before gaseous mixture is got back to hydrogenation zone.Conventionally adopt recycle compressor to increase the pressure of this gas part.Salt in the moisture inorganic process liquid drop that contains residual water-based hydroxyl ammonium salt causes the generation of for example, dirt on recycle compressor (blade), and due to these dirts, the maintenance cost of recycle compressor is higher.In addition, maintenance need to be interrupted recycle compressor, and this can reduce the output of hydroxylammonium production plant, because at maintenance intercourse, the production of hydroxylammonium also can be interrupted.
Detailed Description Of The Invention
Therefore, the object of this invention is to provide a kind of method of preparing hydroxylammonium in successive processes, the alternative known method of the method overcomes the limitation problem of valuable chemical composition loss and the Boundary Limit of hydroxylammonium production plant work output.
Contriver surprisingly finds, the waterborne liquid reclaiming is turned back to the synthetic district of hydroxyl ammonium salt by mist eliminator is installed from mist eliminator simultaneously, can overcome above-mentioned shortcoming, the variable cost that this can reduce maintenance cost and produce hydroxylammonium.Meanwhile, by using mist eliminator, the hydroxylammonium salt being entrained in gaseous mixture can be recovered.Further, the mist leaving in the gaseous mixture of hydrogenation zone is made up of inorganic process liquid drop, the salt that inorganic process liquid comprises water and dissolving, and described salt comprises phosphoric acid salt, nitrate, amine salt and hydroxylammonium salt.The pH value of inorganic process liquid is 1-4(25 ℃). the gross weight mark of the salt dissolving in inorganic process liquid is 25wt%-50wt%.
In addition, an object of the present invention is, compare with the traditional method of implementing in identical production unit, improved the average preformance of hydroxylammonium.With respect to the traditional method of implementing in identical production unit, the method will more be saved.
Therefore, the invention provides a kind of utilize hydrogenation nitrate or oxynitride in hydrogenation reactor continuous production hydroxylammonium to form the method for hydroxylammonium, ammonium, nitrogen and nitrous oxide, described hydrogenation reactor comprises a) mist eliminator, b) plenum zone and c) the synthetic district of hydroxyl ammonium salt, wherein the synthetic district of this hydroxyl ammonium salt comprises that wherein said method comprises the following steps containing the gentle phase of water:
I) collect gas phase at plenum zone;
II) alternatively, spray water drips in collected gas phase;
III) by from step I) the gas phase collected or in Step II) in added water droplet the gas phase of collecting by mist eliminator [B];
IV) from mist eliminator [B], reclaim and contain the liquid that condenses water-containing drop, this water-containing drop contains hydroxyl ammonium salt;
Wherein add at least a portion from step IV to the synthetic district of hydroxyl ammonium salt) the liquid of mist eliminator [B] recovery.
Preferably, Step II) be enforceable.More preferably, the water droplet adding described in is made up of deionized water (also referred to as de-mineralized water) or steam condensate.
Preferably, process of the present invention is
process.Described
process comprises that a hydroxyl ammonium salt synthesizes district, in this synthetic district, in the moisture inorganic process liquid that contains water and phosphoric acid, under the existence of hydrogen at catalyzer, nitrate or nitric oxide reduction is become to azanol.Also can with nitrate ion supplement moisture inorganic process liquid and in this inorganic process liquid partly soluble byproduct ammonia be converted into nitrogen.
Can be any applicable reactor for the preparation of the production unit of hydroxylammonium, for example, there is reactor or the bubble-plate column of mechanical stirrer, more preferably bubble-plate column.NL6908934 has described the example of suitable bubble-plate column.
The typical reactor configurations of preparation water-based hydroxylammonium salt solution and solid catalyst particle is the hydrogenation bubble-column reactor with cooling segment.Reactor configurations usually comprises gas delivery pipe and the strainer tube of a lot of groups.
In method of the present invention, the synthetic district of hydroxyl ammonium salt comprises containing the gentle phase of water.
Described hydrogen, heterogeneous hydrogenation catalyst, the phosphoric acid salt of dissolving and the hydroxylammonium of ammonium and saliferous that contains dissolving containing water.
The described gas phase of leaving the synthetic district of hydroxyl ammonium salt comprises the mist of moisture inorganic process liquid drop.
Fresh hydrogen is input to the synthetic district of hydroxyl ammonium salt in some way by known concentration (hydrogen pressure) own.Preferably, minimum hydrogen partial pressure in synthetic hydroxyl ammonium salt district is maintained at least 0.3MPa.Conventionally, in the synthetic district of hydroxyl ammonium salt average hydrogen partial pressure for being less than 10MPa.
The definition of mist is the drop being entrained in gas.In the present invention, mist is separated into liquids and gases.
Conventionally, mist eliminator is a kind of equipment, and this equipment is installed in gas-liquid separation pipe to improve the removal that is entrained in drop in gas.Described mist eliminator can be that any structure or one can be condensed into mist the cyclone that weight is enough to isolated drop from gas.
Mist eliminator can be made any size and shape by the material of relative broad range, for example plastics, pottery, metal or its alloy.
Mist eliminator operates according to the following step conventionally:
A. contain the gas phase of residual drop by mist eliminator, this gas phase can freely be passed through mist eliminator;
B. described residual drop contact mist eliminator surface cohesion;
C. by be formed at that large cohesion drop in net finally drains and ingress pipe at the bottom of.
Described structure can be from woven wire cloth sheet, plastic mesh sheet, and reticular pattern coalescent filter, selects in foil package or other similar structures.
Preferably, mist eliminator [B] is equipped with a 421Koch-Otto York net or a 431Koch-Otto York net.Preferably, the thickness of net is 0.05-0.75m.
Preferably, mist eliminator is made up of 304L stainless steel.
Preferably, net sheet and grid are made up of 304L stainless steel.
Mist eliminator [B] may be installed on inside or the outside of hydrogenation reactor.If be installed on inside, preferably at the top of plenum zone.This selection requires less use steel in reactor builds.But the maintenance meeting of mist eliminator [B] is more complicated, because whole reactor should carry out degassed and close at that time.
Preferably, be sprayed onto the collection water droplet amount of gas phase and the gaseous phase volume of collection than being 0.001-0.01kg water/Nm
3gas phase is more preferably 0.007-0.05kg water/Nm
3gas phase.
Preferably, be sprayed onto the water droplet amount of collecting gas phase with the volume summation of adding fresh hydrogen and recycle gas (comprising hydrogen) in hydrogenation reactor to than being 0.002-0.08kg water/Nm
3gas is more preferably 0.005-0.05kg water/Nm
3gas phase, is most preferably 0.007-0.045kg water/Nm
3gas.
Preferably, the gas phase of collecting is being 30-70 ℃ by the front temperature of mist eliminator [B].
Preferably, the gas phase of collecting is being 0.5-4MPa by the front pressure of mist eliminator [B].
Preferably, the agglomeration liquid under gravity or pumping action, at least a portion mist eliminator [B] being reclaimed joins the synthetic district of hydroxyl ammonium salt.
Accompanying drawing explanation
As shown in Figure 1, wherein mist eliminator is placed in hydrogenation reactor inside (this figure has only shown reactor top cage structure) to specific embodiment of the invention scheme.
As shown in Figure 2, wherein mist eliminator is placed in hydrogenation reactor outside (this figure does not show reactor) to specific embodiment of the invention scheme.
In the present invention, in hydrogenation reactor, as shown in Figure 3, wherein mist eliminator is positioned at the top of hydrogenation reactor to the specific embodiments of the part process of continuous production hydroxylammonium.
In the present invention, in hydrogenation reactor, as shown in Figure 4 and Figure 5, wherein mist eliminator is positioned at the outside of hydrogenation reactor to the specific embodiments of the part process of continuous production hydroxylammonium.
Fig. 1
In Fig. 1, mist eliminator [B] is arranged on the top in hydrogenation reactor [A].Metal sheet [D] is arranged on the top of hydrogenation reactor [A].Metal sheet [D] comprises 2 holes, and two vertical ductings are welded in respectively in hole.Larger pipeline [E] is positioned at central authorities, collects the gas phase (stream [x]) that contains mist by this pipeline, and this mist contains the moisture inorganic process liquid drop containing hydroxyl ammonium salt, and described gas phase is left the synthetic district of hydroxyl ammonium salt and upwards flowed.Add deionized water by line [2] and atomizer [C] to the gas phase (stream [x]) of this collection.
Liquid is collected at top at metal sheet [D], and the moisture inorganic industrial liquid drop of cohesion of the hydroxyl ammonium salt that this liquid contains mist eliminator [B] recovery is also discharged this agglomeration liquid from less pipeline [F].The agglomeration liquid (stream [y]) that mist eliminator [B] is reclaimed is introduced directly into the synthetic district of hydroxyl ammonium salt of hydrogenation reactor [A].Except mist gas stream [z] is discharged from hydrogenation reactor [A] top.
Fig. 2
In Fig. 2, pipe [G] is furnished with mist eliminator [B].Deionized water adds in the collection gas phase (air-flow [x]) that contains moisture inorganic process liquid drop mist by atomizer [C], and described inorganic process liquid drop contains hydroxyl ammonium salt, and the gas of the free of water droplets of acquisition is through mist eliminator [B].Also discharge as stream [y] agglomeration liquid inflow pipe [G] bottom of reclaiming from mist eliminator [B].Except mist gas stream [z] is discharged from the top of pipe [G].
Fig. 3
In Fig. 3, by line [5], moisture inorganic process liquid is incorporated in hydrogenation reactor [A] and carries out hydrogenation in the synthetic district of hydroxyl ammonium salt simultaneously.Plenum zone at hydrogenation reactor is collected the gas phase containing inorganic process liquid drop mist, and this inorganic process liquid drop contains hydroxyl ammonium salt, and this gas phase flows out by pipeline [E].The structure of described mist eliminator [B] as shown in Figure 1.
Crossing line [3] except mist gas communication discharges and is divided into recycle gas and waste gas.Described recycle gas is the part except mist gas phase, should be added back to hydrogenation reactor [A] by line [3a] and then arrive the synthetic district of hydroxyl ammonium salt except mist gas phase.Described waste gas is discharged by line [3b].The recycle gas obtaining is incorporated into recycle compressor [J] by line [3a], supplements after fresh hydrogen by line [6], and concentrated recycle gas enters in hydrogenation reactor [A].
Be drained in gas-liquid separator [H] by line [8] containing granules of catalyst with from the liquid phase of the gas phase of hydrogenation reactor [A].In gas-liquid separator [H], gas phase and liquid phase separation.The gas phase that gas-liquid separator [H] obtains is got back in hydrogenation reactor [A] by line [9].The liquid phase that gas-liquid separator [H] obtains flows in liquid-solid filter plant [I] by line [10], and the filtrate producing in this filter plant is discharged by line [11].Hydrogenation reactor bottom is discharged and flow into the remaining liquid phase containing granules of catalyst by line [12].
Fig. 4
Hydrogenation reactor described in Fig. 3 [A] is as shown in Figure 4 and have a following difference:
At the plenum zone of hydrogenation reactor [A], can obtain the gas phase (stream [x]) of the collection that contains moisture inorganic process liquid drop mist and discharge by the line [9] that is positioned at reactor head, described inorganic process liquid drop contains hydroxyl ammonium salt.
Discharge by line [9a] gas phase that gas-liquid separator [H] obtains.
In gas phase online [9b] in line [9] and line [9a], merge.By atomizer [C] (not showing, referring to Fig. 2) herein, the deionized water in line [2] is added in the air-flow of described merging.The gas phase of the free of water droplets obtaining enters pipe [G] and passes through mist eliminator [B].Collect the agglomeration liquid containing cohesion inorganic process liquid drop in the bottom of pipe [G], this inorganic process liquid drop contains the hydroxyl ammonium salt being reclaimed by mist eliminator [B] will discharge from the top of pipe [G] except mist air-flow by line [3] simultaneously.Bottom at pipe [G] is discharged the agglomeration liquid of mist eliminator [B] recovery and can (i) be joined in gas-liquid separator [H] by line [4a] by line [4], (ii) join in the line [10] between gas-liquid separator and liquid-solid filter plant [I] by line [4b], (iii) join in liquid-solid filter plant [I] by line [4c], or (iv) join the downstream of liquid-solid filter plant [I] by line [4d].In described embodiment, recovering liquid flows into hydrogenation reactor [A].
Fig. 5
Hydrogenation reactor described in Fig. 3 [A] is as shown in Figure 5 and have a following difference:
At the plenum zone of hydrogenation reactor [A], can obtain the collection gas phase (stream [x]) containing the mist of moisture inorganic process liquid drop and discharge by the line [9] that is positioned at reactor head, described inorganic process liquid drop contains hydroxyl ammonium salt.
Discharge by line [9a] gas phase that gas-liquid separator [H] obtains.In gas phase online [9b] in line [9] and line [9a], merge.By atomizer [C] (not showing, referring to Fig. 2) herein, the deionized water in line [2] is added in the air-flow of described merging.The gas phase of the free of water droplets obtaining enters pipe [G] and passes through mist eliminator [B].
The agglomeration liquid that mist eliminator [B] reclaims is collected in bottom at pipe [G], will discharge from the top of pipe [G] except mist air-flow by line [3] simultaneously.The mist air-flow that removes obtaining is divided into recycle gas and waste gas.Described waste gas is discharged by line [3b].Described recycle gas is incorporated in compressor [J] and is supplemented fresh hydrogen by line [6] simultaneously by line [3a], afterwards concentrated recycle gas is entered in hydrogenation reactor [A].The agglomeration liquid that mist eliminator [B] reclaims bottom at pipe [G] before discharging by line [4] is collected and can be incorporated in line [5] by line [4a], or is introduced directly into the bottom of reactor [A] by line [4b].In such scheme, can use pump the liquid of recovery to be incorporated into the bottom of line [5] or reactor [A] (Fig. 5 does not show).
Further illustrate the present invention by following examples, but be not limited to these embodiment.
Embodiment
?
in equipment, implement embodiment 1,2 and 3, in this equipment, utilize hydrogen, under the effect of Pd/C catalyzer, nitrate selective reduction is become to azanol.In the hydrogenation reactor of bubble-cap tower, carry out the hydrogenation of nitrate.Aqueous liquid phase in bubble-plate column contains the mixture that is mainly ammonium, phosphoric acid salt, nitrate, hydrogen and hydroxylammonium ion.The feed gas of hydrogenation reactor is the mixture of fresh hydrogen and recycle gas.
Embodiment 1
To continuous operation
hydrogenation reactor in equipment adds about 5.2Nm
3/ s gas, this gas is the mixture of fresh hydrogen and recycle gas (comprising hydrogen).Temperature in reactor is 50 ℃, and pressure is 2.2MPa.Pipe [G] is higher than gas-liquid separator [H] (referring to Fig. 4).
Pipe [G] has the mist eliminator that diameter is 1.6m [B] and is equipped with 12 " thick (approximately 0.3m) Koch-Otto York
style421.Net sheet and grid material are to be made up of 304L stainless steel.
Add deionized water by atomizer [C] to the gas phase of collecting [9b], input speed is 0.04kg/s.
The use of mist eliminator can prevent that recycle compressor from keeping in repair because of salt dirt.
To continuous operation
hydrogenation reactor in equipment adds about 4.7Nm
3/ s gas, this gas is the mixture of fresh hydrogen and recycle gas (comprising hydrogen).Temperature in reactor is 50 ℃, and pressure is 2.2MPa.The key distinction of embodiment 1 and embodiment 2 is the pipe position of [G] and the model of mist eliminator [B], referring to Fig. 5.Pipe [G] is lower than gas-liquid separator [H] in the present embodiment.Utilize pump that the recovery salt of aquosity stream is introduced directly in the moisture inorganic process liquid of hydrogenation reactor by line [4] and [4a].Pipe [G] is equipped with 6 " thick (approximately 0.15m) Koch-Otto York
style431 mist eliminator [B].Net sheet and grid material are to be made up of 304L stainless steel.
Enter pipe [G] in gas phase front, add deionized water by atomizer [C], input speed is 0.1kg/s.
The use of mist eliminator can prevent that recycle compressor from being keeped in repair because of salt dirt.
To continuous operation
hydrogenation reactor in equipment adds general 1.8Nm
3/ s gas, this gas is the mixture of fresh hydrogen and recycle gas (comprising hydrogen).Temperature in reactor is 60 ℃, and pressure is 2.7MPa.The upper end of hydrogenation reactor is equipped with mist eliminator [B] (referring to Fig. 3).Add deionized water by atomizer [C] to the gas phase of collecting (stream [x]), input speed is 0.08kg/s.Mist eliminator [B] (York
style421) diameter is 1.6m, 12 " thick (approximately 0.3m).Net sheet and grid material are to be made up of 304L stainless steel.
The use of mist eliminator can prevent that recycle compressor from being keeped in repair because of salt dirt.
Claims (16)
1. continuous production hydroxylammonium is to form a method for hydroxylammonium, ammonium, nitrogen and nitrous oxide in hydrogenation reactor to utilize hydrogenation nitrate or oxynitride, and described hydrogenation reactor comprises a) mist eliminator, b) plenum zone and c) the synthetic district of hydroxyl ammonium salt; Wherein the synthetic district of this hydroxyl ammonium salt comprises that wherein said method comprises the following steps containing the gentle phase of water:
I) collect gas phase at plenum zone;
II) alternatively, spray water drips in collected gas phase;
III) by from step I) the gas phase collected or in Step II) in sprayed water droplet the gas phase of collecting by mist eliminator [B];
IV) from mist eliminator [B], reclaim and contain the liquid that condenses water-containing drop, this water-containing drop contains hydroxyl ammonium salt;
Wherein add at least a portion at step IV to the synthetic district of hydroxyl ammonium salt) in the liquid of mist eliminator [B] recovery.
2. method according to claim 1, wherein in Step II) in, in the gas phase of collecting, spray water droplet.
3. method according to claim 1 and 2, phosphoric acid salt and ammonium and the saliferous hydroxylammonium of the wherein said hydrogen that contains dissolving containing water, heterogeneous hydrogenation catalyst, dissolving.
4. the method described in any one according to claim 1 or 3, the gas phase of wherein leaving the synthetic district of hydroxyl ammonium salt comprises the mist of moisture inorganic process liquid drop.
5. the method described in any one according to claim 1 or 4, the liquid wherein under gravity or pumping action, mist eliminator [B] being reclaimed is incorporated into the synthetic district of hydroxyl ammonium salt.
6. the method described in any one according to claim 1 or 5, wherein said mist eliminator [B] contains a structure or one and mist can be condensed into the cyclone of the drop that weight is enough to separate from gas phase.
7. method according to claim 6, wherein said structure can from woven wire cloth sheet, plastic mesh sheet, reticular pattern coalescent filter and or foil package select.
8. method according to claim 6, wherein structure is net sheet.
9. method according to claim 8, wherein net sheet is made up of 304L stainless steel.
10. according to the method described in claim 1-9 any one, the water droplet amount that is wherein sprayed onto gas phase with the volume summation of adding fresh hydrogen and recycle gas (comprising hydrogen) in hydrogenation reactor to than being 0.002-0.08kg water/Nm
3gas.
11. according to the method described in claim 1-10 any one, and the gas phase of wherein collecting is being 30-70 ℃ by the front temperature of mist eliminator [B].
12. according to the method described in claim 1-11 any one, and the gas phase of wherein collecting is being 0.5-4MPa by the front pressure of mist eliminator [B].
13. according to the method described in claim 1-12 any one, and wherein mist eliminator [B] is equipped with 421Koch-Otto York net or 431Koch-Otto York net.
14. according to the method described in claim 1-13 any one, and wherein mist eliminator [B] is installed on hydrogenation reactor outside.
15. according to the method described in claim 1-13 any one, and wherein mist eliminator [B] is installed on the top in hydrogenation reactor.
16. according to the method described in claim 1-15 any one, and wherein said water droplet is made up of deionized water or steam condensate.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1418809A (en) * | 2002-12-11 | 2003-05-21 | 中国石油化工股份有限公司巴陵分公司 | Method for prepn. of high concentration hydroxymaline in the prodn. process of hexanolactam |
| CN201529409U (en) * | 2009-10-27 | 2010-07-21 | 中国石油化工股份有限公司 | Gas-liquid mass transfer device |
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| CN102671470A (en) * | 2012-05-23 | 2012-09-19 | 浙江大学 | Efficient gas-liquid separator |
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- 2013-12-02 CN CN201310632164.1A patent/CN103848406A/en active Pending
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| CN1418809A (en) * | 2002-12-11 | 2003-05-21 | 中国石油化工股份有限公司巴陵分公司 | Method for prepn. of high concentration hydroxymaline in the prodn. process of hexanolactam |
| CN201529409U (en) * | 2009-10-27 | 2010-07-21 | 中国石油化工股份有限公司 | Gas-liquid mass transfer device |
| CN202237589U (en) * | 2011-10-21 | 2012-05-30 | 神华集团有限责任公司 | Rotary cutting type demister, coal gas diffusion water seal with rotary cutting type demister, and tower with rotary cutting type demister |
| CN102671470A (en) * | 2012-05-23 | 2012-09-19 | 浙江大学 | Efficient gas-liquid separator |
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