CN109011700A - A kind of Liquid liquid Separation device and a kind of method for preparing diphenylmethane series diamines and polyamines - Google Patents
A kind of Liquid liquid Separation device and a kind of method for preparing diphenylmethane series diamines and polyamines Download PDFInfo
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- CN109011700A CN109011700A CN201810699878.7A CN201810699878A CN109011700A CN 109011700 A CN109011700 A CN 109011700A CN 201810699878 A CN201810699878 A CN 201810699878A CN 109011700 A CN109011700 A CN 109011700A
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- knockout drum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/68—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
- C07C209/78—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton from carbonyl compounds, e.g. from formaldehyde, and amines having amino groups bound to carbon atoms of six-membered aromatic rings, with formation of methylene-diarylamines
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Abstract
The present invention relates to a kind of Liquid liquid Separation device and a kind of methods for preparing diphenylmethane series diamines and polyamines.Liquid liquid Separation device mainly includes horizontal knockout drum, vertical knockout drum and corresponding filler unit, and the Combination Design of horizontal knockout drum is added using vertical knockout drum, avoids the defect of single horizontal tank or vertical tank equipment of itself structure；Horizontal tank feed pipe is designed using insertion tube, and designs tubaeform outer cover in nozzle, and vertical knockout drum feeding line is fed using horizontal direction, and big flow is avoided to feed the impact to layering interfaces；Separative efficiency is further increased by designing the means such as different coalescent pack layers again.Liquid liquid Separation device of the present invention is applied in the preparation of diphenylmethane series diamines and polyamines, the phase separation stability of intermediate product is greatly improved, and reduce water phase components content in organic phase, thereby reduces later separation workshop section energy consumption.
Description
Technical field
The invention belongs to MDI preparation and separation technology field, it is related to a kind of Liquid liquid Separation device and a kind of prepares diphenyl
The method of methane series diamines and polyamines.
Background technique
The diamines and polyamines (abbreviation DAM) of diphenylmethane series are understood to refer to the mixing of following kind of amine and amine
Object:
Wherein n indicates >=0 natural number.It in form can be by replacing all NH of compound of formula with NCO group2Group
Obtained from corresponding isocyanates, be accordingly called diisocyanate, the diphenylmethane series of diphenylmethane series
Polyisocyanates or or diphenylmethane series diisocyanate and polyisocyanates (MDI).
According to the prior art, it is related at least three liquid-liquid diphase separation process during the preparation process, including will react and obtain
Acid neutralize after mixture be separated into thick polyamines phase and crude salt water phase, by the mixture point after the washing of thick polyamines organic phase
From for the smart polyamines phase comprising aniline and water and including aniline, the water phase etc. of polyamines.The above-mentioned polyamines that obtains mutually is passed through into distillation
Aniline and water are removed, and is further separated into aniline phase and water phase by the way that aniline and aqueous mixtures will be isolated.
EP1652835 A1, page 3, the 58th row to 2103595 A1 of the 13rd row and EP of page 4, page 7, the 21st to 37
Row, discloses prior art routine post-processing approach.1652835 A1 of EP teach in and with after subsequent wash, water phase
It will receive the considerably damage of the third phase to be formed (impurity or impurity layer) from the separation process in the organic phase containing product.It should
Third phase be it is stable, hinder and mutually separate, extreme there are a large amount of interphase between water phase and organic phase sometimes
In the case of even prevent and mutually separate.In some cases, this also results in continuous production and is forced to interrupt.In operating process
In the worst case, it is necessary to by the complete emptying of one or more phase separation containers and clean, and discarded content or to its into
Row post-processing.Even if the organic phase for avoiding the formation of impurity layer, but obtaining after separation of the phases still includes significant percentage of aqueous
Ingredient can increase substantially the energy consumption of later separation in further processing steps.Therefore during preparing polyamines
The separating effect for improving liquid-liquid diphase has important value.
Improve two-phase laminated flow efficiency reduce intermediate course many methods be it is known, have both at home and abroad at present numerous patents with
This technology is related, if 2008/148631 A1 of WO describes a kind of condensation process, by using containing 0.001% (quality)
Divalent/multivalent metal cation formalin, to avoid the formation of middle layer.2103595 A1 of EP discloses this and mutually separates
Problem can be carried out by addition water and/or aniline, and provide a kind of preferred embodiment, will be dilute by addition water and/or aniline
The reaction mixture released is divided into organic phase and water phase in Florence formula (Florentine) flask with partition.Above-mentioned two
Piece patent improves separative efficiency by way of adding auxiliary agent or other components into reaction product, but adding auxiliary agent can not
The process flow of the subsequent polyamines of extension and salt refining workshop section that avoid, and increase separating energy consumption.Even if can be to avoid
The formation (such as result of the measure described in 2008/148631 A1 of EP 1652835 A1 and WO) of impurity layer, but in phase
Organic phase obtained after separation still may include significant percentage of water composition as dispersed phase, in further process step
In will lead to similar problem, to generate the impurity layer of entrainment.Patent CN201480033234.4 is referred to by two-phase
Increase the method for coarse separation equipment after crude separation to improve separative efficiency, but this method increase process flows and equipment to throw
Money.
It is relatively simple for structure in existing liquid liquid horizontal phase splitter, the cylinder in mostly simple cavity.Nozzle is fed in phase-splitter
Side center, organic phase material nozzle and lower layer's material nozzle are respectively in the upper and lower part of phase-splitter, while in inducer
Bottom also sets up discharging hole, and live liquidometer nozzle is arranged in end.Material enters phase-splitter by feed inlet, and mixed material is because of density
Difference is gradually layered in phase-splitter, and more past the right feed separation time is longer, and layered effect is better, can finally be divided on the right
From.The shortcomings that this phase-splitter, is: when processing larger flow material, because material charging rate is higher, directly impacting phase-splitter
Material is easy to interfere material layering, influences the split-phase effect of phase-splitter, and then affects subsequent separation, increases and is produced into
This.It is simultaneously to ensure that material has enough residence times in phase-splitter, it usually needs large volume of phase-splitter is increased and set
Standby investment.
As it can be seen that in existing literature in cited and description DAM preparation process, it is main by addition auxiliary agent, increase secondary
The means such as separation equipment improve separative efficiency, lack a kind of simple and effective separation means to improve liquid-liquid diphase in production process
Separative efficiency, interstitial impurity layer during two-phase laminated flow is reduced, to improve production stability, while will be after separation in organic phase
Watr-proportion and separation after organic Phase Proportion in water phase minimize, to reduce the production cost of prior art.
Summary of the invention
Aiming at the above shortcomings existing in the prior art, the present invention provides a kind of Liquid liquid Separation device, separative efficiency Gao Shi
It is wide with range, and other auxiliary agent impurity are not introduced, for can significantly mention in the preparation of diphenylmethane series diamines and polyamines
Liquid-liquid diphase separative efficiency in high DAM production, improving production stability reduces production cost.
The present invention also provides a kind of methods for preparing diphenylmethane series diamines and polyamines, i.e., in the phase of intermediate product
Above-mentioned Liquid liquid Separation device is used in separation process, separation process stability is greatly improved, and reduce water in organic phase
Phase component content, to further reduced later separation workshop section energy consumption.
Technical solution of the present invention is as follows:
A kind of Liquid liquid Separation device, including horizontal knockout drum and vertical knockout drum；
The horizontal knockout drum, one end are equipped with feed pipe, and it is light group positioned at tank body upper wall that the other end, which is set there are two outlet,
Sub-export is heavy constituent outlet positioned at tank body lower wall；In tank body, tubaeform outer cover is installed in feed pipe exit, into
Level-one rough segmentation coalescent pack layer is set between expects pipe and two outlet and second level segments coalescent pack layer；
The vertical knockout drum is successively arranged top coalescent pack layer, light component feed pipe, recombination in tank body from top to bottom
Divide feed pipe and lower part coalescent pack layer；
The light fraction outlet of the horizontal knockout drum, recombination sub-export respectively with the light component feed pipe of vertical knockout drum,
Heavy constituent feed pipe is connected；
The vertical knockout drum, tank deck are equipped with light component discharge nozzle, and tank bottom is equipped with heavy constituent discharge nozzle.
Further, the feed pipe, light component feed pipe, heavy constituent feed pipe are horizontal insertion tube.
Further, the tubaeform outer cover, depth are that feed pipe is inserted into the 60~90% of horizontal separation canister length, preferably
70~80%；The tubaeform housing opening is located at big opening end, and opening direction is with feed pipe export direction on the contrary, tubaeform outer cover
Big mouth bore, osculum bore and horizontal knockout drum internal diameter ratio be 0.6~0.8:0.2~0.4:1；Horn opening angle is
20 °~80 °, preferably 30 °~50 °, more preferable 45 °；Tubaeform outer cover is fixed on horizontal knockout drum cylinder inboard wall by supporting element
On.
Further, the level-one rough segmentation coalescent pack layer, bed horizontal direction width are the 10 of horizontal separation canister length
~20%, packing layer vertical direction total height is 50~80%, preferably the 60~70% of horizontal knockout drum internal diameter.
The level-one rough segmentation coalescent pack layer is the V-type corrugated plating of one group of parallel arrangement, and plate spacing is 10~60cm, excellent
Select 20~30cm, preferably 90 °~150 ° of V-shaped groove opening angle；The V-type corrugated plating plate face is parallel to tank body central axis, cross
To setting in horizontal knockout drum.
Preferably, the V-type corrugated plating material is 304 stainless steels by tungsten carbide modification, method of modifying are as follows:
Plate surface additional layer is with a thickness of 10~25 μm of tungsten carbide coating；Modified surface roughness (Ra) range is 0.4~3.2
μm, preferably 0.8~1.6 μm.It is modified by increasing tungsten carbide coating in baffle surface, suitable rough surface can be obtained
Degree, significantly improves dispersed phase in the rate of adsorption of packing layer sheet metal surface.
Further, the second level segments coalescent pack layer, and bed width is the 10~20% of horizontal separation canister length；Bed
Layer porosity is 77~89%, preferably 79~85%, more preferable 82~84%.
The second level segments coalescent pack layer, and material is the wire packing made of cohesive fiber；The cohesive fiber
Diameter is 1~100 μm, preferably 1~50 μm, more preferable 10~20 μm.
The cohesive fiber is the mixing with different surfaces property fiber；It is preferred that tri acetic acid fiber cellulose fiber, 316L are golden
Belonging to the mixing of fiber and polyacrylonitrile resin fiber, mass percentage group becomes cellulose triacetate fiber 20~40%,
It is preferred that 25~30%, 316L metallic fiber 30~60%, preferably 40~50%, polyacrylonitrile resin fiber 25~45%, preferably
30~40%, amount to 100%.The surface property of coalescence material is a key factor for influencing separative efficiency, is mainly reflected in
Influence of the wetability of fiber surface to the demulsification absorption and collision coalescence process of drop, due to the complexity of oil mixing with water physical performance
Property, the fiber of single surface property tends not to satisfy the use demand, using can with the mixing establishment of different surfaces performance fibers
Obtain suitable fiber surface performance.
Further, the top coalescent pack layer is 316L wire mesh packing, and coalescent pack layer in lower part is polypropylene
Nitrile wire packing；
The top coalescent pack layer and lower part coalescent pack layer, bed porosity are 77~89%, preferably 79~
85%, more preferable 82~84%.Thickness of bed layer is the 5~20% of vertical tank vertical height, preferably 10~15%.
Further, the light component feed pipe outlet installation light component feeding spray nozzle, heavy constituent feed pipe outlet installation
Heavy constituent feeding spray nozzle, light component feeding spray nozzle and the outlet of heavy constituent feeding spray nozzle are horizontal direction.
A method of the diamines and polyamines preparing diphenylmethane series are to be related to the process of water-oil phase separation
In, using the above-mentioned Liquid liquid Separation device of the present invention, mixed material is separated into organic phase and water phase.
Preferably, the method for the diamines and polyamines for preparing diphenylmethane series is by aniline and formaldehyde in acid
Condensation reaction is carried out under catalytic action, is obtained the diamines and polyamines (abbreviation DAM) of diphenylmethane series, is used in the method
The water-oil phase separation process of above-mentioned Liquid liquid Separation device includes: the mixed material after the acid for obtaining condensation reaction neutralizes
It is separated into thick polyamines organic phase and crude salt water phase；Mixed material after the washing of thick polyamines organic phase is separated into comprising aniline and water
Smart polyamines organic phase and the water phase comprising aniline, polyamines etc.；The smart polyamines organic phase comprising aniline and water is obtained by above-mentioned
Aniline and water are separated by distillation, the mixed material of the aniline separated and water is further separated into aniline organic phase and water phase.
Further, using the water-oil phase separation process of above-mentioned Liquid liquid Separation device, step includes:
1) mixed material enters horizontal knockout drum by feed pipe, is changed by tubaeform outer cover and is flowed to, and reduces mixed material
Middle drop flow velocity in the horizontal direction, while accelerating the flow velocity of vertical direction, then carried out by level-one rough segmentation coalescent pack layer
Initial gross separation carries out secondary separation using second level subdivision coalescent pack layer, is separated into heavy constituent (organic phase) and light group
Divide (water phase), horizontal knockout drum is discharged by recombination sub-export and light fraction outlet respectively；
2) light component and heavy constituent of step 1) discharge pass through light component feed pipe and heavy constituent feed pipe level side respectively
It to the vertical knockout drum of entrance, and is uniformly distributed in the horizontal direction, while a small amount of heavy constituent drop of light component entrainment is on top
It is settled after mutual collision coalescence in coalescent pack layer, a small amount of light component drop carried secretly in heavy component is in lower part coalescent pack layer
It floats after mutual collision coalescence, water phase is discharged to obtain by tank deck light component discharge nozzle in the light component after separation, and heavy constituent is by tank bottom weight
Organic phase is discharged to obtain in component discharge nozzle.
The above-mentioned method for preparing diphenylmethane series diamines and polyamines, specifically includes the following steps:
(a) aniline and formaldehyde carry out condensation reaction in the presence of acidic catalysts, obtain comprising diphenylmethane series
The reaction mixture of diamine salts and polyamines salt,
(b) alkali is added in the reaction mixture of above-mentioned diphenylmethane series diamine salts and polyamines salt and neutralize instead
It answers,
(c) reaction system from step (b) is divided into thick polyamines organic phase and crude salt water phase in Liquid liquid Separation device,
(d) the water phase washing purifying for obtaining thick polyamines organic phase obtained in step (c) using step (g),
(e) mixture obtained in step (d) is divided into the smart polyamines comprising aniline and water in Liquid liquid Separation device has
Machine phase and water phase comprising aniline, polyamines etc.,
(f) water and aniline are removed in a manner of distillation from the smart polyamines organic phase in step (e), obtains purification
DAM product,
(g) by the aniline and aqueous mixtures that remove in step (f) be separated into Liquid liquid Separation device aniline organic phase and
Water phase, aniline organic phase circulation is as the part material reacted in step (a), and water phase is for the washing in step (d).
Preferably, in step c), separation temperature is 70~130 DEG C, preferably 90~110 DEG C；In step e), separation temperature is
70~130 DEG C, preferably 90~110 DEG C；In step g), separation temperature is 5~50 DEG C, preferably 10~25 DEG C.
The thick polyamines organic phase mass percentage composition obtained in step c) is as follows: DAM content 65~80%, aniline
Content 12~27%, water content about 3~3.5%.
The essence polyamines organic phase component percentages obtained in step e) are as follows: containing 1~8.5% water, and according to
The proportion of aniline and formaldehyde, the DAM containing 5~50%, preferably 5~30% aniline and 10~80%, preferably 50~70%.
The composition of the aniline organic phase mass percentage obtained in step g) is as follows: aniline content 86%-~90%, water
Content 10~10.5%.
Technical solution of the present invention beneficial effect is:
Liquid liquid Separation device of the present invention is a kind of new and effective continuous liquid-liquid two phase stratification equipment, using vertical knockout drum
The Combination Design for adding horizontal knockout drum avoids the defect of single horizontal tank or vertical tank equipment of itself structure；Horizontal tank charging
Pipe is designed using insertion tube, and designs tubaeform outer cover in nozzle, and vertical knockout drum feeding line is fed using horizontal direction, kept away
Exempt from impact of the big flow charging to layering interfaces；Separation effect is further increased by designing the means such as different coalescent pack layers again
Rate.Liquid liquid Separation device of the present invention is applied in the preparation of diphenylmethane series diamines and polyamines, intermediate production is greatly improved
The phase separation stability of object, separation process reduce water phase components content in organic phase without interphase, thereby reduce
Later separation workshop section energy consumption.
Detailed description of the invention
Fig. 1 is 1 Liquid liquid Separation apparatus structure schematic diagram of embodiment；
In Fig. 1: 1, horizontal knockout drum, 2, vertical knockout drum, 11, feed pipe, 12, light fraction outlet, 13, recombination separate
Mouthful, 14, tubaeform outer cover, 15, level-one rough segmentation coalescent pack layer, 16, second level subdivision coalescent pack layer, 21, top coalescent pack
Layer, 22, light component feed pipe, 23, heavy constituent feed pipe, 24, lower part coalescent pack layer, 25, light component discharge nozzle, 26, recombination
Separate expects pipe, 27, light component feeding spray nozzle, 28, heavy constituent feeding spray nozzle；
Fig. 2 is V-type partition position schematic diagram in level-one rough segmentation coalescent pack layer；
In Fig. 2: 1, V-type corrugated plating, 2, horizontal knockout drum tank skin.
Specific embodiment
Technical solution of the present invention and its advantages are further illustrated with reference to the accompanying drawings and embodiments.
Embodiment 1
A kind of Liquid liquid Separation device, as shown in Figure 1, including the horizontal knockout drum 1 and vertical knockout drum being connected to by pipeline
2；
Horizontal knockout drum 1, one end are equipped with feed pipe 11, and it is light group positioned at tank body upper wall that the other end, which is set there are two outlet,
Sub-export 12 is heavy constituent outlet 13 positioned at tank body lower wall；In tank body, tubaeform outer cover is installed in 11 exit of feed pipe
14, level-one rough segmentation coalescent pack layer 15 and second level subdivision coalescent pack layer 16 are provided between feed pipe 11 and two outlets；
Vertical knockout drum 2 is successively arranged top coalescent pack layer 21, light component feed pipe 22, again in tank body from top to bottom
Component feed pipe 23 and lower part coalescent pack layer 24；The outlet of light component feed pipe 22 installation light component feeding spray nozzle 27, heavy constituent
Feed pipe 23, which exports, installs heavy constituent feeding spray nozzle 28, and the nozzle of light component feeding spray nozzle 27 and heavy constituent feeding spray nozzle 28 is
Horizontal direction；Tank deck is equipped with light component discharge nozzle 25, and tank bottom is equipped with heavy constituent discharge nozzle 26；
The light fraction outlet 12 of horizontal knockout drum 1, recombination sub-export 13 are separately connected the light component charging of vertical knockout drum 2
Pipe 22, heavy constituent feed pipe 23.
Feed pipe 11, light component feed pipe 22, heavy constituent feed pipe 23 are horizontal insertion tube.
The tubaeform opening of outer cover 14 is located at big opening end, and opening direction is with 11 export direction of feed pipe on the contrary, tubaeform outer cover
It is fixed on by supporting element on the cylinder inboard wall of horizontal knockout drum 1.
Level-one rough segmentation coalescent pack layer 15, is the V-type corrugated plating of one group of parallel arrangement, and V-type corrugated plating plate face is parallel to tank
Body central axis is transversely mounted in horizontal knockout drum 1 (Fig. 2).V-type corrugated plating material is surface additional layer with a thickness of 15 μm
Tungsten carbide coating 304 stainless steel plates, surface roughness (Ra) be 1.5 μm.
Top coalescent pack layer 21 is 316L wire mesh packing, and bed porosity is 83.5%, and thickness of bed layer is vertical
The 13.5% of tank vertical height.Lower part coalescent pack layer 24 is polyacrylonitrile wire packing, and bed porosity is 83.5%, bed
With a thickness of the 13.5% of vertical tank vertical height.
Embodiment 2
A method of diphenylmethane series diamines and polyamines system is prepared, using the Liquid liquid Separation device of embodiment 1,
In:
Tubaeform 14 depth of outer cover is that feed pipe 11 is inserted into the 65% of horizontal 1 length of knockout drum；Tubaeform outer cover 14 it is big
Mouth bore is the 0.7% of horizontal 1 internal diameter of knockout drum；Horn opening angle is 45 °.
Level-one rough segmentation coalescent pack layer 15, bed horizontal direction width are the 10% of horizontal 1 length of knockout drum, and layer is square vertically
To 50% that total height is horizontal 1 internal diameter of knockout drum.
V-type corrugated plating, plate spacing 10cm, 120 ° of V-shaped groove opening angle.
Second level segments coalescent pack layer 16, and bed porosity is 77%, and material is that the silk screen made of cohesive fiber is filled out
Material；The cohesive fiber diameter is 10 μm.Cohesive fiber is tri acetic acid fiber cellulose fiber, 316L metallic fiber and polyacrylonitrile tree
The mixing of rouge fiber, mass percentage group become cellulose triacetate fiber 20%, 316L metallic fiber 40%, polypropylene
Nitrile resin fibre 40%.
Specific steps are as follows: (a) aniline (mass concentration 94%) and formaldehyde (mass concentration 37%) are in acidic catalyst hydrochloric acid
Condensation reaction is carried out in the presence of (mass concentration 32%), obtains the reaction comprising diphenylmethane series diamine salts and polyamines salt
Mixture, reaction time 60min, 50~103 DEG C of reaction temperature；(b) alkali is added to above-mentioned diphenylmethane series diamine salts
With carry out neutralization reaction in the reaction mixture of polyamines salt, caustic soda additional amount is to neutralize the hydrochloric acid the desired amount of 120% being added；
(c) reaction system from step (b) is divided into thick polyamines organic phase and crude salt water phase in Liquid liquid Separation device of the invention,
Separation temperature is 90~110 DEG C；(d) thick polyamines organic phase obtained in step (c) is washed using the water phase that step (g) obtains
Purifying；(e) mixture obtained in step (d) is divided into the smart polyamines organic phase comprising aniline and water in Liquid liquid Separation device
And the water phase comprising aniline, polyamines etc., separation temperature are 90~110 DEG C；(f) in a manner of distillation by water and aniline from step
(e) it is removed in the smart polyamines organic phase in, obtains the DAM product of purification；(g) aniline and water that remove in step (f) are mixed
Object is separated into aniline organic phase and water phase in Liquid liquid Separation device, and separation temperature is 10~25 DEG C, and aniline organic phase circulation is made
For the part material reacted in step (a), water phase is for the washing in step (d)；
Step (c), step (e), water content is as shown in table 1 in the organic phase that step (g) is isolated.
The Liquid liquid Separation device prepared using above-described embodiment 1, is separated into water phase and organic phase, separation side for mixed material
Method are as follows:
1) mixed material enters horizontal knockout drum 1 by plug-in type feed pipe 11 in the horizontal direction, passes through tubaeform outer cover 14
Change mixed material flow direction, horizontal direction flow velocity is greatly lowered, reduces the impact to two-phase interface, while increasing mixed material
Middle light component and heavy constituent promote water-oil phase further to separate in the flow velocity of vertical direction.Mixed material goes successively to one
Grade rough segmentation coalescent pack layer 15 carries out initial gross separation of water-oil phase, partition by the modified V-type corrugated plating of tungsten carbide surface
Presence increase the turbulent extent of liquid, improve the probability that contacts with each other of dispersed phase, while by carrying out to baffle surface
It is modified, enhance dispersed phase drop in the absorption property of baffle surface, dispersed phase drop constantly takes off after baffle surface coalescence increases
From；Mixture by partition rough segmentation travels further into second level subdivision coalescent pack layer 16, and cohesive fiber bed has different tables
The material of face activity energy adsorbs dispersed phase drop of different nature respectively, and dispersed phase drop is constantly intercepted by cohesive fiber, adsorbed,
It is detached from fiber surface in gravity after droplet coalescence increases to a certain degree, carries out sedimentation separation.It is thin by cohesive fiber bed
It is divided into heavy constituent (organic phase) and light component (water phase), horizontal separation is discharged by recombination sub-export 13 and light fraction outlet 12 respectively
Tank；
2) light component and heavy constituent pass through light component feed pipe 22 and heavy constituent feed pipe 23 respectively, are fed by light component
Spray head 27 and 28 horizontal direction of heavy constituent feeding spray nozzle enter vertical knockout drum, and are uniformly distributed in the horizontal direction, while light
A small amount of heavy constituent drop of component entrainment settles after mutual collision coalescence in top coalescent pack layer 21, carries secretly in heavy component
A small amount of light component drop floats after mutual collision coalescence in lower part coalescent pack layer 22, and the light component after separation is by light group of tank deck
It separates expects pipe 25 and water phase is discharged to obtain, organic phase is discharged to obtain by tank bottom heavy constituent discharge nozzle 26 in heavy constituent.
Embodiment 3
A method of diphenylmethane series diamines and polyamines system is prepared, using the Liquid liquid Separation device of embodiment 1,
In:
Tubaeform 14 depth of outer cover is the 75% of 11 intubating length of feed pipe；The big mouth bore of tubaeform outer cover 14 is horizontal
The 70% of 1 internal diameter of knockout drum, horn opening angle are 45 °.
Level-one rough segmentation coalescent pack layer 15, bed overall thickness are the 15% of horizontal 1 length of knockout drum, and layer total height is horizontal
The 65% of 1 internal diameter of knockout drum.V-type corrugated plating, plate spacing 30cm, 75 ° of V-shaped groove opening angle.
Second level segments coalescent pack layer 16, and bed porosity is 83%.
Specific steps with embodiment 2, the difference is that: in step (c), separation temperature be 90~110 DEG C；Step (e)
In, separation temperature is 90~110 DEG C；In step (g), separation temperature is 10~25 DEG C.
Mixed material is separated into the separation method of water phase and organic phase also with embodiment 2.Step (c), step (e), step
Suddenly water content is as shown in table 1 in the organic phase that (g) is isolated.
Comparative example 1
It is carried out under conditions of same as Example 2, the difference is that: used Liquid liquid Separation device is single horizontal point
Layer tank, the single coalescent pack unit of internal use, material selection 316L wire mesh, 15 μm of fibre diameter, porosity 80%,
Separation process is there are interphase, step (c), step (e), and water content is as shown in table 1 in the organic phase that step (g) is isolated.
Comparative example 2
It is carried out under conditions of same as Example 2, the difference is that: second level segments coalescent pack layer in horizontal knockout drum
Using single coalescent pack unit, material selection 316L wire mesh, 15 μm of fibre diameter, porosity 80%, step
(c), step (e), water content is as shown in table 1 in the organic phase that step (g) is isolated.
Comparative example 3
It is carried out under conditions of same as Example 2, the difference is that: level-one rough segmentation coalescent pack layer in horizontal knockout drum
The V-type corrugated plating material used is 304 stainless steel of non-modified processing, step (c), step (e), what step (g) was isolated
Water content is as shown in table 1 in organic phase.
Comparative example 4
It is carried out under conditions of same as Example 2, the difference is that: it only include this hair in used Liquid liquid Separation device
Bright horizontal knockout drum and its internal structure, step (c), step (e), water content such as 1 institute of table in the organic phase that step (g) is isolated
Show.
Comparative example 5
It is carried out under conditions of same as Example 2, the difference is that: it only include this hair in used Liquid liquid Separation device
Bright vertical knockout drum and its internal structure, step (c), step (e), water content such as 1 institute of table in the organic phase that step (g) is isolated
Show.
Water content/wt% in 1 organic phase of table
| The thick polyamines organic phase of step (c) | Step (e) essence polyamines organic phase | Step (g) aniline organic phase | |
| Embodiment 2 | 3.5 | 8.3 | 10.5 |
| Embodiment 3 | 3.0 | 8.0 | 10.2 |
| Comparative example 1 | 4.6 | 10.3 | 13.5 |
| Comparative example 2 | 4.0 | 9.1 | 12.3 |
| Comparative example 3 | 3.8 | 8.5 | 12 |
| Comparative example 4 | 4.3 | 9.8 | 13.2 |
| Comparative example 5 | 5.0 | 12.0 | 14.0 |
Claims (10)
1. a kind of Liquid liquid Separation device, it is characterised in that: including horizontal knockout drum and vertical knockout drum；
The horizontal knockout drum, one end are equipped with feed pipe, and it is that light component goes out positioned at tank body upper wall that the other end, which is set there are two outlet,
Mouth is heavy constituent outlet positioned at tank body lower wall；In tank body, tubaeform outer cover is installed in feed pipe exit, in feed pipe
Level-one rough segmentation coalescent pack layer is set between two outlets and second level segments coalescent pack layer；
The vertical knockout drum, be successively arranged in tank body from top to bottom top coalescent pack layer, light component feed pipe, heavy constituent into
Expects pipe and lower part coalescent pack layer；
The light fraction outlet of the horizontal knockout drum, recombination sub-export respectively with the light component feed pipe of vertical knockout drum, recombination
Feed pipe is divided to be connected；
The vertical knockout drum, tank deck are equipped with light component discharge nozzle, and tank bottom is equipped with heavy constituent discharge nozzle.
2. Liquid liquid Separation device according to claim 1, it is characterised in that:
The feed pipe, light component feed pipe, heavy constituent feed pipe are horizontal insertion tube；
The tubaeform outer cover, depth are that feed pipe is inserted into 60~90%, preferably the 70~80% of horizontal separation canister length；
The tubaeform housing opening is located at big opening end, opening towards with feed pipe export direction on the contrary, tubaeform outer cover it is big
Mouth bore and horizontal knockout drum internal diameter ratio are 0.6~0.8:1；Horn opening angle be 20 °~80 °, preferably 30 °~50 °,
More preferable 45 °.
3. Liquid liquid Separation device according to claim 1, it is characterised in that:
The level-one rough segmentation coalescent pack layer, bed horizontal direction width are the 10~20% of horizontal separation canister length, packing layer
Vertical direction total height is 50~80%, preferably the 60~70% of horizontal knockout drum internal diameter；
The level-one rough segmentation coalescent pack layer, be one group of parallel arrangement V-type corrugated plating, plate spacing be 10~60cm, preferably 20
~30cm, preferably 90 °~150 ° of V-shaped groove opening angle, the V-type corrugated plating plate face is parallel to tank body central axis, laterally sets
It sets in horizontal knockout drum.
4. Liquid liquid Separation device according to claim 3, it is characterised in that: the V-type corrugated plating material is by carbonization
304 stainless steels of tungsten modification, method of modifying are as follows: applied in plate surface additional layer with a thickness of 10~25 μm of tungsten carbide
Layer；Modified surface roughness Ra range is 0.4~3.2 μm, preferably 0.8~1.6 μm.
5. Liquid liquid Separation device according to claim 1, it is characterised in that:
The second level segments coalescent pack layer, and bed horizontal direction width is the 10~20% of horizontal separation canister length；Bed hole
Gap rate is 77~89%, preferably 79~85%, more preferable 82~84%；
The second level segments coalescent pack layer, and material is the wire packing made of cohesive fiber；The cohesive fiber diameter
It is 1~100 μm, preferably 1~50 μm, more preferable 10~20 μm.
6. Liquid liquid Separation device according to claim 5, it is characterised in that:
The cohesive fiber is the mixing of the fiber with different surfaces property；It is preferred that tri acetic acid fiber cellulose fiber, 316L metal
The mixing of fiber and polyacrylonitrile resin fiber, mass percentage group becomes cellulose triacetate fiber 20~40%, excellent
Select 25~30%, 316L metallic fiber 30~60%, preferably 40~50%, polyacrylonitrile resin fiber 25~45%, preferably 30
~40%, amount to 100%.
7. Liquid liquid Separation device according to claim 1, it is characterised in that:
The top coalescent pack layer is 316L wire mesh packing, and coalescent pack layer in lower part is polyacrylonitrile wire packing；
The top coalescent pack layer and lower part coalescent pack layer, bed porosity are 77~89%, and preferably 79~85%, more
It is preferred that 82~84%, thickness of bed layer is the 5~20% of vertical tank vertical height, preferably 10~15%.
8. Liquid liquid Separation device according to claim 1, it is characterised in that: light group of light component feed pipe outlet installation
Divide feeding spray nozzle, heavy constituent feed pipe outlet installation heavy constituent feeding spray nozzle, light component feeding spray nozzle and heavy constituent feeding spray nozzle
Outlet is horizontal direction.
9. a kind of method for the diamines and polyamines for preparing diphenylmethane series, it is characterised in that: be to be related to water-oil phase
During separation, using any one of the claim 1~8 Liquid liquid Separation device, by mixed material be separated into organic phase and
Water phase.
10. according to the method described in claim 9, it is characterized by: the water-oil phase using above-mentioned Liquid liquid Separation device separates
Process, step include:
1) mixed material enters horizontal knockout drum by feed pipe, is changed by tubaeform outer cover and is flowed to, and then passes through level-one rough segmentation
Coalescent pack layer carries out an initial gross separation, carries out secondary separation using second level subdivision coalescent pack layer, is separated into heavy constituent
And light component, horizontal knockout drum is discharged by recombination sub-export and light fraction outlet respectively；
2) step 1) discharge light component and heavy constituent pass through respectively light component feed pipe and heavy constituent feed pipe horizontal direction into
Enter vertical knockout drum, while a small amount of heavy constituent drop of light component entrainment sinks after mutual collision coalescence in top coalescent pack layer
It drops, a small amount of light component drop carried secretly in heavy component floats after mutual collision coalescence in lower part coalescent pack layer, after separation
Water phase is discharged to obtain by tank deck light component discharge nozzle in light component, and organic phase is discharged to obtain by tank bottom heavy constituent discharge nozzle in heavy constituent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810699878.7A CN109011700B (en) | 2018-06-29 | 2018-06-29 | Liquid-liquid separation device and method for preparing diphenylmethane series diamine and polyamine |
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| CN201810699878.7A CN109011700B (en) | 2018-06-29 | 2018-06-29 | Liquid-liquid separation device and method for preparing diphenylmethane series diamine and polyamine |
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