CN208791523U - A kind of purification alpha-pyrrolidone steams the device of slag - Google Patents
A kind of purification alpha-pyrrolidone steams the device of slag Download PDFInfo
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- CN208791523U CN208791523U CN201821604821.6U CN201821604821U CN208791523U CN 208791523 U CN208791523 U CN 208791523U CN 201821604821 U CN201821604821 U CN 201821604821U CN 208791523 U CN208791523 U CN 208791523U
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- pyrrolidone
- slag
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Abstract
The utility model provides a kind of device of purification alpha-pyrrolidone steaming slag, including rectifying column, and rectifying column includes tower reactor, lower tower section and upper tower section, steams slag feed(raw material)inlet and selective solvent feed mouth wherein being provided on lower tower section side wall；The upper end of upper tower section is connected with exteenal reflux distillation tower head, exteenal reflux distillation tower head side connects spiral condenser, first vacuum orifice is set above spiral condenser, lower section is arranged condensate liquid and collects diversion pipe, fraction receiving tank is connected below diversion pipe, the second vacuum orifice is arranged in fraction receiving tank top side port, and light phase condensate liquid refluxing opening is arranged in middle part side port, return pipe is set on light phase condensate liquid refluxing opening, and return pipe is connected by pipeline with exteenal reflux distillation tower head.The device that the utility model structure alpha-pyrrolidone that is simple, easy to operate, extracting is with high purity, quality is good, recovery rate is high, low energy consumption and the purification alpha-pyrrolidone of large-scale production is suitble to steam slag.
Description
Technical field
The utility model belongs to the extractive technique field of active principle in fine chemistry industry waste material, more particularly, to a kind of purification
The device of alpha-pyrrolidone steaming slag.
Background technique
Alpha-pyrrolidone, colourless crystallization, 245 DEG C of boiling point, can be dissolved in water, alcohol, ether, chloroform, benzene, acetic acid by 24.6 DEG C of fusing point
The majority organic solvent such as ethyl ester and carbon disulfide, is mainly used for synthesizing important medicine intermediate n-vinyl pyrrolidone.Mesh
The widest method that preceding production n-vinyl pyrrolidone uses is exactly alpha-pyrrolidone and acetylene in certain temperature and pressure
Under power, formed by catalyst preparation of alkali.The conversion ratio of the method alpha-pyrrolidone only has 65%-80% at present, in addition can also
The impurity for generating 5-15%, tower reactor can obtain the steaming slag of 10-20% after causing n-vinyl pyrrolidone to refine.
Steaming slag composition is sufficiently complex, and containing dozens to hundreds of kind of component, wherein the most component of content is unreacted α-
Pyrrolidones, therefore also referred to as alpha-pyrrolidone steams slag, the other impurity steamed in slag have 1,4-butanediol, gamma-butyrolacton, N- first class pyrrole
Pyrrolidone, 3- methyl pyrrolidone, 4- methyl pyrrolidone and tetramethylpiperidinol etc., they are waved relatively with alpha-pyrrolidone
Hair degree very little, direct rectifying can not obtain high-purity alpha-pyrrolidone product, and the alpha-pyrrolidone color that direct rectifying obtains
For yellow, it is not able to satisfy the demand of downstream production.Overwhelming majority n-vinyl pyrrolidone manufacturer selects this portion at present
Divide steaming slag charge directly to burn, gives process units heat supply as the energy.This scheme not only because steam a large amount of nitride in slag there are due to
It pollutes the environment, the loss for steaming alpha-pyrrolidone material in slag charge but will be caused.
Have to mention in disclosed patent adds water to be crystallized into the alpha-pyrrolidone containing impurity, obtains high-purity α-pyrroles
Alkanone product.The method is only applicable to that the dopant species in alpha-pyrrolidone are single and content is less, alpha-pyrrolidone content compared with
High situation.Also some will steam slag be dissolved in water, be sufficiently stirred after filter, then the mode of mother liquor rectifying is obtained into high-purity α-pyrroles
Alkanone.But the method is suitable only for the separation of alpha-pyrrolidone and vinyl pyrrolidone polymer, to property and boiling point and α-
The separating effect that the close liquid of pyrrolidones steams slag is bad.
Summary of the invention
In view of this, the utility model is directed to a kind of device of purification alpha-pyrrolidone steaming slag, structure is simple, easily grasps
The alpha-pyrrolidone make, extracted is with high purity, quality is good, recovery rate is high, low energy consumption and is suitble to purification α-pyrroles of large-scale production
The device of alkanone steaming slag.
In order to achieve the above objectives, the technical solution of the utility model is achieved in that
A kind of purification alpha-pyrrolidone steams the device of slag, including rectifying column, rectifying column include tower reactor, lower tower section and upper tower
Section steams slag feed(raw material)inlet and selective solvent feed mouth wherein being provided on lower tower section side wall；The upper end of upper tower section is connected with outer
Flow back distillation tower head, and exteenal reflux distillation tower head side connects spiral condenser, and setting first is taken out true above spiral condenser
It eats dishes without rice or wine, lower section is arranged condensate liquid and collects diversion pipe, and fraction receiving tank, the setting of fraction receiving tank top side port are connected below diversion pipe
Second vacuum orifice, middle part side port are arranged light phase condensate liquid refluxing opening, return pipe, return pipe are arranged on light phase condensate liquid refluxing opening
It is connected by pipeline with exteenal reflux distillation tower head.
Further, lower tower section and upper tower section are provided with filler, and filler is that θ shape, triangle spiral shape or spring shape dissipate landfill
Material.Filler size is 4 × 4mm of Φ, 5 × 5mm of Φ.
Further, gas phase temperature detection mouth is arranged in exteenal reflux distillation tower head top.
Further, upper tower section and lower tower section height and diameter ratio are 15-20:1.Ratio of height to diameter is excessive to will lead to production pressure drop
Become larger, production cost becomes larger.The too small alpha-pyrrolidone product quality that will lead to output of ratio of height to diameter is not high.
Further, it vacuumizes and is vented by three-way valve control at the second vacuum orifice.
Further, fluid-tight is carried out using U-tube between light phase condensate liquid refluxing opening and exteenal reflux distillation tower head, avoids gas
Phase materials directly cause loss of material from return pipe extraction.
Further, it steams on slag feed(raw material)inlet, selective solvent feed mouth and light phase condensate liquid refluxing opening and is respectively provided with cock
Valve.It steams slag raw material and selective solvent is all made of peristaltic pump charging, peristaltic pump feed rate is stablized, can effectively be avoided because of flow
Fluctuation lead to occur in tower liquid flooding and other chain reactions.
Further, vacuum jacket is provided on the outside of exteenal reflux distillation tower head, the external use of upper tower section and lower tower section is poly-
Urethane insulating tube is kept the temperature.
Working principle:
Refine the method that alpha-pyrrolidone steams slag, comprising the following steps:
(1) liquid level at selective solvent to light phase condensate liquid refluxing opening will be added in fraction receiving tank, from snakelike pipework condensation
Device and fraction receiving tank vacuumize simultaneously, by selective solvent and alpha-pyrrolidone steam slag raw material by 1:1 from selective solvent into
Material mouth and steaming slag feed(raw material)inlet are pumped into rectifying column, carry out rectification under vacuum, collect fraction in fraction receiving tank；By fraction receiving tank
Position purpose is to prevent the initial stage of driving at interior addition selective solvent to light phase condensate liquid refluxing opening, leads in tower without reflux
It causes the alpha-pyrrolidone product quality situation not up to standard of extraction to occur, vacuumizes and refer to and vacuumize the operating pressure in system
To 5-10kpa, prevent heat-sensitive substance from issuing biochemical variation in the higher environment of temperature.
(2) it after the liquid level in fraction receiving tank is higher than light phase condensate liquid refluxing opening, opens at light phase condensate liquid refluxing opening
Plug valve, light phase selective solvent is back in rectifying column, at the same keep boundary position height it is constant under the premise of, by nothing
Color heavy phase fraction is produced from mouth under fraction receiving tank；Boundary position height is constant in holding fraction receiving tank needs to adjust fraction receiving tank
Lower mouth valve opening continuously produces heavy phase fraction alpha-pyrrolidone with certain rate；
(3) when alpha-pyrrolidone content is less than 1% in the kettle liquid of analysis tower reactor, it is continuous to start alpha-pyrrolidone steaming slag raw material
Charging, while kettle liquid interval produces, the selective solvent that the kettle liquid of discharge is isolated after split-phase returns to be continued to make in rectifying column
With.Slag continuously only is steamed into alpha-pyrrolidone after kettle liquid qualified, is because selective solvent recycles in system from beginning to end
And do not produce, so not needing to supplement.
Further, alpha-pyrrolidone steams the content 30-65% of alpha-pyrrolidone in slag raw material.
Further, selective solvent is fat hydrocarbon.Preferably, selective solvent is the aliphatic saturated hydrocarbon of C12-C14
Class.
Further, the mode of operation that the device that purification alpha-pyrrolidone steams slag uses is light phase infinite reflux, and heavy phase is adopted entirely
Out.
Further, rectifying column uses high vacuum azeotropic distillation.
Compared with the existing technology, the device that purification alpha-pyrrolidone described in the utility model steams slag has the advantage that
The device that purification alpha-pyrrolidone described in the utility model steams slag passes through control fraction receiving tank circle position height
The reflux of mode control selections solvent and the extraction of alpha-pyrrolidone product, control means are simple, and fractional composition is stablized, and are not necessarily to
The additional reflux ratio for increasing reflux pump or the independent control system of electromagnetic relay, pendulum；By using high vacuum condition to α-pyrrole
Pyrrolidone steams slag raw material and is refined, and avoids steaming the temperature-sensitive impurity in slag material by way of reducing system operating temperature in essence
The case where chemically reacting during system, cause security risk appearance；The selective solvent dosage of use is few, and solvent is in object
It is not produced in material subtractive process, is recycled in system always, without doing many deposits, can be effectively reduced being produced into for enterprise
This.
Detailed description of the invention
The attached drawing for constituting a part of the utility model is used to provide a further understanding of the present invention, this is practical new
The illustrative embodiments and their description of type are not constituteed improper limits to the present invention for explaining the utility model.?
In attached drawing:
Fig. 1 is the structural schematic diagram for the device that purification alpha-pyrrolidone steams slag described in the utility model embodiment.
Description of symbols:
1- tower reactor；Tower section under 2-；The upper tower section of 3-；4- steams slag feed(raw material)inlet；5- selective solvent feed mouth；6- exteenal reflux essence
Evaporate tower head；7- gas phase temperature detection mouth；8- spiral condenser；9- fraction receiving tank；10- condensate liquid collects diversion pipe；11- is light
Phase condensate liquid refluxing opening；The first vacuum orifice of 12-；The second vacuum orifice of 13-.
Specific embodiment
It should be noted that in the absence of conflict, the feature in the embodiments of the present invention and embodiment can
To be combined with each other.
In the description of the present invention, it should be understood that term " center ", " longitudinal direction ", " transverse direction ", "upper", "lower",
The orientation or positional relationship of the instructions such as "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside" is
It is based on the orientation or positional relationship shown in the drawings, is merely for convenience of describing the present invention and simplifying the description, rather than indicate
Or imply that signified device or element must have a particular orientation, be constructed and operated in a specific orientation, therefore cannot understand
For limitations of the present invention.In addition, term " first ", " second " etc. are used for description purposes only, and should not be understood as indicating
Or it implies relative importance or implicitly indicates the quantity of indicated technical characteristic." first ", " second " etc. are defined as a result,
Feature can explicitly or implicitly include one or more of the features.It is in the description of the present invention, unless another
It is described, the meaning of " plurality " is two or more.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " is pacified
Dress ", " connected ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integrally
Connection；It can be mechanical connection, be also possible to be electrically connected；Can be directly connected, can also indirectly connected through an intermediary,
It can be the connection inside two elements.For the ordinary skill in the art, on being understood by concrete condition
State the concrete meaning of term in the present invention.
The utility model will be described in detail below with reference to the accompanying drawings and embodiments.
As shown in Figure 1, a kind of purification alpha-pyrrolidone steams the device of slag, including rectifying column, rectifying column include tower reactor 1, under
Tower section 2 and upper tower section 3 steam slag feed(raw material)inlet 4 and selective solvent feed mouth 5 wherein being provided on lower 2 side wall of tower section；Upper tower section
3 upper end is connected with exteenal reflux distillation tower head 6, and 6 side of exteenal reflux distillation tower head connects spiral condenser 8, snakelike pipework condensation
First vacuum orifice 12 is set above device 8, and lower section is arranged condensate liquid and collects diversion pipe 10, and connection fraction receives below diversion pipe 10
The second vacuum orifice 13 is arranged in tank 9,9 top side port of fraction receiving tank, and light phase condensate liquid refluxing opening 11, light phase is arranged in middle part side port
Condensate liquid refluxing opening 11 is connected by pipeline with exteenal reflux distillation tower head 6.
Above-mentioned lower tower section 2 and upper tower section 3 are provided with filler, and filler is θ shape, triangle spiral shape or spring shape random packing.
Gas phase temperature detection mouth 7 is arranged in above-mentioned 6 top of exteenal reflux distillation tower head.
Above-mentioned upper tower section 3 and lower 2 height of tower section and diameter ratio are 15-20:1.
It vacuumizes and is vented by three-way valve control at above-mentioned second vacuum orifice 13.
It is attached between above-mentioned light phase condensate liquid refluxing opening 11 and exteenal reflux distillation tower head 6 for U-tube.
Plug valve is respectively provided on above-mentioned steaming slag feed(raw material)inlet 4, selective solvent feed mouth 5 and light phase condensate liquid refluxing opening 11
Door.
Vacuum jacket is provided on the outside of above-mentioned exteenal reflux distillation tower head 6, upper tower section 3 and the external of lower tower section 2 use poly- ammonia
Ester insulating tube is kept the temperature.
Working principle:
Selective solvent will be added in fraction receiving tank 9 to 11 position of middle part light phase liquid refluxing opening, then from coiled pipe
Second vacuum orifice 13 of 8 top of condenser and the first vacuum orifice 12 of fraction receiving tank 9 vacuumize simultaneously, are pressed with peristaltic pump
1:1 volume ratio is pumped into alpha-pyrrolidone respectively and steams slag raw material and selective solvent to the 2/3 of the total liquid level of tower reactor.Spiral condenser
8 are passed through cooling medium from entrance, have fraction extraction in later on heating device to fraction receiving tank 9, with fraction receiving tank 9
Liquid level gradually rises to 11 or more light phase condensate liquid refluxing opening, opens the plug valve at light phase condensate liquid refluxing opening 11, opens
The reflux of beginning light phase is increased to the light phase condensate liquid refluxing opening 11 and fraction receiving tank 9 at 9 middle part of fraction receiving tank to weight phase interface
Lower mouth spacing 1/2 when, open 9 bottom of fraction receiving tank heavy phase produce valve, start produce alpha-pyrrolidone product, lead to
Crossing control valve aperture remains unchanged phase interface position in fraction receiving tank 9, entire refining system stable operation.
Purification alpha-pyrrolidone employed in following embodiment steams slag raw material sources in Hebei company, by simply de-
Light treated material, wherein each component content (mass fraction) is respectively as follows: alpha-pyrrolidone 62.62%, azeotropic impurity
3.35%, heavy seeds 34.03%.Following embodiment is all made of the device that purification alpha-pyrrolidone of the present invention steams slag.Raw material,
The detection device that fraction and kettle liquid use is FL9790II type gas chromatograph, nonpolar 60m capillary column.
Embodiment 1
Total high 1.5m of selection diameter 30mm, lower tower section 2 and upper tower section 3 is tested, and is pumped into 2L tower reactor 1 and is steamed slag original
Expect that 700ml, selective solvent n-dodecane 700ml, operating pressure 10kpa carry out rectification under vacuum.The bottom temperature of rectifying column
124.6 DEG C, 113.9 DEG C of tower top temperature, lower leaf is carried out in fraction receiving tank 9, upper layer is solvent phase, and lower layer is heavy phase.It adopts
With upper layer solvent phase infinite reflux, the mode of operation that lower layer's fraction produces entirely, split-phase volume ratio light phase: heavy phase=10:1, gas phase color
Spectrum detects alpha-pyrrolidone content 99.91% in lower layer's fraction of extraction, and selective solvent residual quantity is 87ppm in fraction, evaporates
Point color is that other indexs such as colourless, smell and transparency are all satisfied requirements of the national standard.Continue extraction to tower top α-pyrrolidines
When ketone content is less than 99.9%, chromatography detects tower reactor alpha-pyrrolidone content 0.78%, at this time heavy phase recovery ratio 61.66%.
Embodiment 2
The rectifying column that the total height of selection diameter 30mm, lower tower section 2 and upper tower section 3 is 1.5m is tested, to 2L tower reactor 1
In be pumped into steam slag raw material 700ml, selective solvent n-tridecane 700ml, operating pressure 10kpa rectification under vacuum, the tower of rectifying column
154.0 DEG C of kettle temperature degree, 143.9 DEG C of tower top temperature, lower leaf is carried out in fraction receiving tank 9, upper layer is solvent phase, and lower layer attaches most importance to
Phase, split-phase volume ratio light phase: heavy phase=5.5:1, gas chromatographic detection extraction lower layer's fraction in alpha-pyrrolidone content
99.91%, selective solvent residual quantity is 66ppm in fraction, and fraction color is that other indexs such as colourless, smell and transparency are equal
Meet requirements of the national standard.When continuing to produce to tower top alpha-pyrrolidone content less than 99.9%, chromatography detects tower reactor α-pyrroles
Alkanone content 0.81%, at this time heavy phase recovery ratio 60.82%.
Embodiment 3
The rectifying column that the total height of selection diameter 50mm, lower tower section 2 and upper tower section 3 is 2m is tested, and is pumped to 5L tower reactor 1
Enter to steam slag raw material 1500ml, selective solvent n-tridecane 1500ml, operating pressure 10kpa rectification under vacuum, the tower reactor of rectifying column
153.8 DEG C of temperature, lower leaf is carried out in fraction receiving tank 9, adopts upper layer solvent phase infinite reflux, lower layer by 142.9 DEG C of tower top temperature
The mode of operation that fraction produces entirely, split-phase volume ratio light phase: heavy phase=5.2:1, gas chromatographic detection extraction lower layer's fraction in
Alpha-pyrrolidone content 99.92%, selective solvent residual quantity is 67ppm in fraction, and fraction color is colourless, smell and transparent
Other indexs such as degree are all satisfied requirements of the national standard.When continuing to produce to tower top alpha-pyrrolidone content less than 99.9%, chromatography
Tower reactor alpha-pyrrolidone content 0.84% is detected, at this time heavy phase recovery ratio 60.88%.
Comparative example 1
The rectifying column that the total height of selection diameter 30mm, lower tower section 2 and upper tower section 3 is 1.5m is tested, 2L tower reactor pump
Enter to steam slag raw material 1400ml, operating pressure 1-2kpa rectification under vacuum, 161.3 DEG C of the bottom temperature of rectifying column, tower top temperature 115.2
DEG C, the extraction of reflux ratio 50 5%, alpha-pyrrolidone 95.44% in fraction, impurity content 4.56%；Reflux ratio 5 continues to produce
15%, alpha-pyrrolidone 92.88% in fraction, impurity content 7.12%, and fraction color is yellow, product purity, color,
Downstream production requirement is not satisfied in smell.
Comparative example 2
The rectifying column that the total height of selection diameter 30mm, lower tower section 2 and upper tower section 3 is 1.5m is tested, 2L tower reactor pump
Enter to steam slag raw material 700ml, selective solvent n-dodecane 700ml, operating pressure 10kpa rectification under vacuum, the tower reactor temperature of rectifying column
124.6 DEG C of degree, 113.9 DEG C of tower top temperature, reflux ratio 0.5 produces fraction, split-phase volume ratio light phase: heavy phase=10:1, gas phase color
Spectrum detects alpha-pyrrolidone content 99.91% in lower layer's fraction of extraction, and selective solvent residual quantity is 87ppm in fraction, when
Light phase fraction produces 600ml, and when heavy phase fraction produces 60ml, kettle temperature is increased to 162.2 DEG C, and alpha-pyrrolidone contains in heavy phase fraction
Amount is pumped into solvent continuation rectifying again and consumes solvent altogether when alpha-pyrrolidone content is less than 1% in kettle liquid less than 99.9%
6600ml。
As can be seen from the above-described embodiment, by using method purification purification α-pyrroles of selective solvent high vacuum rectification
The content that alpha-pyrrolidone steams alpha-pyrrolidone in slag can be reduced to 1% hereinafter, overhead extraction simultaneously by the method that alkanone steams slag
Alpha-pyrrolidone fraction color be it is colourless, purity be greater than 99.9%, reach the standard requirements of pharmaceutical industry.And the present invention selects
Selective solvent have selectivity high, the few advantage of dosage.
The above is only the preferred embodiment of the utility model only, is not intended to limit the utility model, all at this
Within the spirit and principle of utility model, any modification, equivalent replacement, improvement and so on should be included in the utility model
Protection scope within.
Claims (8)
1. it is a kind of purification alpha-pyrrolidone steam slag device, it is characterised in that: including rectifying column, rectifying column include tower reactor (1), under
Tower section (2) and upper tower section (3) steam slag feed(raw material)inlet (4) and selective solvent feed mouth wherein being provided on lower tower section (2) side wall
(5)；The upper end of upper tower section (3) is connected with exteenal reflux distillation tower head (6), and it is cold that exteenal reflux distillation tower head (6) side connects coiled pipe
The first vacuum orifice (12) are arranged in condenser (8), spiral condenser (8) top, and lower section is arranged condensate liquid and collects diversion pipe (10),
Fraction receiving tank (9) are connected below diversion pipe (10), the second vacuum orifice (13) are arranged in fraction receiving tank (9) top side port, in
Light phase condensate liquid refluxing opening (11) are arranged in portion's side port, and light phase condensate liquid refluxing opening (11) passes through pipeline and exteenal reflux distillation tower head
(6) it is connected.
2. the device that purification alpha-pyrrolidone according to claim 1 steams slag, it is characterised in that: lower tower section (2) He Shangta
Section (3) is provided with filler, and filler is θ shape, triangle spiral shape or spring shape random packing.
3. the device that purification alpha-pyrrolidone according to claim 1 steams slag, it is characterised in that: exteenal reflux distillation tower head
(6) top setting gas phase temperature detection mouth (7).
4. the device that purification alpha-pyrrolidone according to claim 1 steams slag, it is characterised in that: upper tower section (3) He Xiata
Saving (2) is highly 15-20:1 with diameter ratio.
5. the device that purification alpha-pyrrolidone according to claim 1 steams slag, it is characterised in that: the second vacuum orifice (13)
Place is vacuumized and is vented by three-way valve control.
6. the device that purification alpha-pyrrolidone according to claim 1 steams slag, it is characterised in that: light phase condensate liquid refluxing opening
(11) it is attached between exteenal reflux distillation tower head (6) for U-tube.
7. the device that purification alpha-pyrrolidone according to claim 1 steams slag, it is characterised in that: steaming slag feed(raw material)inlet (4),
Plug valve is respectively provided on selective solvent feed mouth (5) and light phase condensate liquid refluxing opening (11).
8. the device that purification alpha-pyrrolidone according to claim 1 steams slag, it is characterised in that: exteenal reflux distillation tower head
(6) outside is provided with vacuum jacket, and the outside of upper tower section (3) and lower tower section (2) uses polyurethane thermal pipe to be kept the temperature.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109096169A (en) * | 2018-09-29 | 2018-12-28 | 天津科林泰克科技有限公司 | A kind of purification alpha-pyrrolidone steams the device and method of slag |
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2018
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109096169A (en) * | 2018-09-29 | 2018-12-28 | 天津科林泰克科技有限公司 | A kind of purification alpha-pyrrolidone steams the device and method of slag |
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