CN202892944U - Evaporator of distillation kettle for distilling dioctyl terephthalate (DOTP) - Google Patents

Evaporator of distillation kettle for distilling dioctyl terephthalate (DOTP) Download PDF

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Publication number
CN202892944U
CN202892944U CN 201220617681 CN201220617681U CN202892944U CN 202892944 U CN202892944 U CN 202892944U CN 201220617681 CN201220617681 CN 201220617681 CN 201220617681 U CN201220617681 U CN 201220617681U CN 202892944 U CN202892944 U CN 202892944U
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heating
kettle
dotp
chamber
evaporimeter
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Expired - Fee Related
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CN 201220617681
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Chinese (zh)
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韩冬
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BEYINFLEX CHEMICALS (SHANGHAI) Co Ltd
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BEYINFLEX CHEMICALS (SHANGHAI) Co Ltd
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Abstract

The utility model relates to an evaporator of a distillation kettle for distilling dioctyl terephthalate (DOTP). The evaporator, an evaporation chamber and a sedimentation chamber are arranged inside a kettle body of the distillation kettle, wherein the evaporation chamber is located above the evaporator, and the sedimentation chamber is located below the evaporator; the top of the kettle body is provided with an upper end enclosure which is communicated with the interior of the kettle body; and the upper end enclosure is provided with a gas phase opening. The evaporator is characterized by comprising a tubular heating jacket and a heating pipe, wherein the tubular heating jacket is continuously distributed along the inner wall of the kettle body, and the heating pipe is coaxially arranged in the kettle body; and heating cavities which are isolated from each other and are only used for flowing through heat conduction oil are respectively formed in the heating pipe and the heating jacket, each heating cavity is communicated with the outside respectively through an oil inlet pipe and an oil outlet pipe, and a heating chamber communicated with the evaporation chamber and the sedimentation chamber is formed by a region located between the heating pipe and the heating jacket. The evaporator of the distillation kettle for distilling DOTP has the advantage that the key technical problems in the preparation of DOTP from PTA (Terephthalic Acid) wastes in industrial production are solved through an innovative structural design of the evaporator.

Description

A kind of evaporimeter that distills the distillation still of DOTP
Technical field
The utility model relates to technical field of chemical, relates in particular to a kind of evaporimeter that is applicable to utilize the distillation still of the distillation DOTP that the prepared DOTP (DOTP) of trade waste be rich in terephthalic acid (TPA) (PTA) purifies.
Background technology
Plasticizer is for increasing its plasticity, flowability and making finished product have the material that pliability adds when processing high polymer (such as rubber, plastics, coating etc.) moulding.DOTP (DOTP) is a kind of main plastic plasticizer of function admirable, except plasticizing capacity a little less than the dioctyl phthalate (DOP), volatility, specific insulation, and the aspect such as the compatibility of PVC and heatproof weatherability more superior, and toxicity is significantly less than DOP.DOTP is mainly used in heatproof 7O ℃ CABLE MATERIALS, and because its volatility is low, use contains quantitative DOTP and can satisfy the requirement of wire cable material temperature resistant grade fully, reaches IEC (IEC), is used as first-selected plasticizer and uses in PVC plastic cable sheath.Its plasticizer that also can be used as other plastics uses, artificial leather film for example, nitrile rubber, cellulose nitrate, polyvinyl butyral etc.In addition, DOTP all has application at paint, paper, lubricant, bidirectional thin, blood plasma poly-bag and handicraft, and prospect is very wide.
Suitability for industrialized production DOTP mainly adopts raw material terephthalic acid (TPA) (PTA) and the preparation of 2-Ethylhexyl Alcohol (isooctanol, octanol) esterification at present.Raw material PTA is the lower end product of petrochemical industry, is a kind of comparatively expensive industrial chemicals, and the DOTP price that this preparation method produces is higher.
In addition, the at present application of PTA is more concentrated, and the PTA more than 90% is for the production of PETG (terylene) in the world.In the production process of terylene, can produce a large amount of discarded objects, those discarded objects enter in the wastewater disposal basin after the peracid dissolving, form the biosolid waste (being designated hereinafter simply as the PTA waste material) that is rich in PTA.These PTA waste materials are difficult to degraded, and as not processing the impact that can cause on the mankind's living environment very severe, processing then needs to drop into a large amount of funds, has increased the production cost of enterprise.
The scheme that exists in the prior art some to utilize above-mentioned PTA waste material to synthesize DOTP; adopt scheme that the PTA waste material prepares DOTO not only raw material be easy to get; simultaneously can digest refuses a large amount of in the industrial production; turn waste into wealth; reduced production cost; but also protection of the environment, be current comparatively rationally and one of the approach of the high recycling of economic benefit.
The scheme that a kind of feasible PTA waste material prepares DOTO be after the PTA that will reclaim purifies through alkalization elimination impurity again acidifying drying to generate purer PTA, and then with the synthetic DOTP plasticizer of original technique, the pre-treatment step of this scheme is various, cost is higher, and owing to the multistep processing has reduced final yield.
In addition, interimly disclosed a kind of " reclaiming the new technology that PTA produces the cable plasticizer " in 2010 05 at public publication publication " living beings Chemical Engineering ", this industrial design concept is the PTA waste material to be carried out after the preliminary treatment dehydration directly and octanol reacts, and will react more afterwards the generation product and carry out purifying products acquisition DOTP.Adopt this technique can avoid all multi-steps such as the purified alkalization that brings of raw material, purification, acidifying, drying, the separation of all impurity is all removed in purifying products, the technical process step that this method is produced DOTP is few, easy to operate, be easy to produce, and product quality is good.
But above-mentioned technique only in the laboratory by experiment vessel carry out operational processes, in the suitability for industrialized production preparation process of reality, need to use distillation still and carry out distilation, distillation still comprises the kettle of pot type, be provided with heat(ing) coil in the described kettle, during work pending material is introduced in the kettle, heated by described heat(ing) coil, thereby reach the purpose of distillation.But common terylene manufacturer produces the PTA waste material and processes as chemical industry rubbish, and for saving processing cost, most producer employs the environmental protection company that processes chemical industry rubbish on behalf of disposal, therefore actual obtainable PTA waste material composition complex not only in the suitability for industrialized production, and be rich in a large amount of solid matters such as silt.The reaction that existing distillation still structure can't be used for this PTA waste material and octanol generates the distillation processing of product, so need to improve to realize above-mentioned preparation scheme for the structure of existing distillation still.
The utility model content
The purpose of the utility model embodiment is for the structural blank of prior art, proposes a kind of evaporimeter that is applicable to distill the distillation still of utilizing the prepared DOTP of PTA waste material.
In order to reach above-mentioned utility model purpose, a kind of evaporimeter that distills the distillation still of DOTP that the utility model embodiment proposes is achieved through the following technical solutions:
A kind of evaporimeter that distills the distillation still of DOTP, related distillation still kettle inside has evaporimeter, be positioned at the vaporization chamber of described evaporimeter top and the mud chamber that is positioned at described evaporimeter below, be provided with a upper cover with described kettle internal communication on the described kettle top, offer gas phase mouth on the described upper cover, bottom, described mud chamber is provided with drainage conduit, it is characterized in that: described evaporimeter comprises along the tubulose heating jacket of described inner wall of kettle continuous distributed and the coaxial heating tube that is arranged in the described kettle, form respectively the heating chamber that only circulates for conduction oil of mutually isolation in described heating tube and the heating jacket, each heating chamber is in communication with the outside by oil inlet pipe and flowline respectively, and the zone between described heating tube and heating jacket consists of and described vaporization chamber, the heating clamber that the mud chamber is communicated with.
The oil-in of described oil inlet pipe is positioned at the bottom of described heating chamber inwall, and the oil-out of described flowline is positioned at the top of described heating chamber inwall.
Described oil-in and described oil-out are respectively formed at the both sides of described heating chamber.
The external diameter of described heating tube is the 15-30% of described kettle internal diameter.
The internal diameter of described heating jacket is the 65-80% of described kettle internal diameter.
Compared with prior art, the beneficial effects of the utility model are: evaporation structure design by novelty has solved PTA waste material in the large-scale industrial production and has prepared key technical problem among the DOTP.The distillation still that proposes in the technical program is applicable to octanol and only processes through alkalization, the distillation of reaction product of PTA waste material behind the drying and processing, realizes extracting in the distillation of complex mixture in suitability for industrialized production the operation of DOTP.It is more easy and economical that the production technology of utilizing this distillation still is processed first the method for synthesizing afterwards at present, and the product properties all meets the requirement of use, for the development of DOTP provides new approach.
Description of drawings
By the description of its exemplary embodiment being carried out below in conjunction with accompanying drawing, the above-mentioned feature and advantage of the utility model will become apparent and easily understand.
Fig. 1 is the utility model embodiment distillation still structural representation;
Fig. 2 is the utility model embodiment distillation still cross-sectional view;
Fig. 3 is that the present embodiment distillation still is looked up structural representation;
Fig. 4 is the present embodiment distillation still demister top view;
Fig. 5 is the present embodiment distillation still demister structural representation;
Fig. 6 is the structural representation of monolithic ripple net sheet in the present embodiment demister.
The specific embodiment
Below in conjunction with accompanying drawing the utility model is described in further detail, so that technical staff's of the same trade understanding:
Shown in Fig. 1-6, label represents respectively:
Kettle cover 1, demister 2, anti-overflow hat 3, anti-overflow ring 4, communication port 5, observation window 6, heating jacket 7, mud chamber 8, drainage conduit 9, heating chamber 10, heating tube 11, heating clamber 12, leg 13, vaporization chamber 14, upper cover 15, gas phase mouth 16, tube connector 17, liquid-inlet 18, housing 19, ripple net sheet 20, pivoted arm 21, screw rod 22;
Oil inlet pipe: a1, a2;
Flowline: a3, a4;
Temperature-measuring port: c1, c2, c3.
Shown in Fig. 1-2, a kind of distillation still that is applicable to utilize the prepared DOTP purification of PTA waste material is provided in the present embodiment, just as described in the background art, owing to entering composition complex in the liquid-solid mixed stocker in the distillation still, even the PTA waste material of institute of same producer output also can produce certain otherness.Cannot also there is no need in this case to carry out qualitative processing for itself and the reacted product of octanol.Just because of this, for the various performances of distillation still strict requirement has been proposed, for example:
Because high boiling product complicated component in the liquid-solid mixed stocker is therefore much higher than existing distillation still for the required precision of the temperature in the distillation still, the slightly poor purity of cut that will cause of its temperature difference control is inadequate.
Because this liquid-solid mixed stocker solid impurity is more, be very easy to deposition or fouling on evaporimeter in still when using conventional distillation still, and then cause the coefficient of overall heat transmission to reduce, temperature in the kettle descends, and the distillation amount reduces in the unit interval, is forced to frequent maintenance cleaning.
Same because the complicated component of liquid-solid mixed stocker, raw material reaction speed has sizable fluctuation after causing heating, even exothermic heat of reaction between the part composition, cause temperature in the kettle pressure sharply to rise, therefore in case control the improper accident that will cause material to go out.
Just for these reasons, the distillation still that provides in the present embodiment mainly is made of kettle, upper cover 15, evaporimeter, erosion control materials device and demister 2, and wherein heater comprises that evaporimeter and mud chamber's heater consist of.Below will the design feature of said modules be described in detail:
Kettle mainly is comprised of three parts: columned kettle body, the still that is located at kettle body upper end pushes up and arranges at the bottom of the still of kettle body lower end, the still top is the semiellipsoid shape, is cone shape at the bottom of the still, and combination encloses space for the heating material distillation of formation with kettle.Kettle inside is provided with the evaporimeter that arranges near upper limb at the bottom of the still, and the still space that is positioned at described evaporimeter top consists of vaporization chamber 14, and the still space that is positioned at described evaporimeter below consists of mud chamber 8.The shape of mud chamber 8 is defined by described still Bottom Shape, and the bottom of mud chamber 8 offers drainage conduit 9, and the high boiling component after being used for distilling is discharged.In addition, autoclave body bottom is provided with the liquid-inlet 18 that is communicated with the mud chamber, for convey materials in still.
The upper cover 15 coaxial tops that are arranged on described still top, and cylindrical, and the lower ending opening of upper cover 15 is communicated with the kettle inner space, expands around the upper end open end to be set as flange.Be equipped with kettle cover 1 on this upper end open end, similarly be formed with the flange that matches for upper cover 15 flanges around the kettle cover 1.Syndeton between kettle cover 1 and the upper cover 15 as shown in Figure 1, be hinged with a pivoted arm 21 that rotates along vertical plane on the sidewall of upper cover 15, this pivoted arm 21 is roughly L-shaped, its transverse arm is pivoted in the primary importance of upper cover 15 sides with between the second place directly over the upper cover 15, and offers screw on the end of this transverse arm (the namely free end of pivoted arm 21).When pivoted arm 21 turns to the second place, the vertical also axis of corresponding described upper cover 15 that arranges of this screw.The center of kettle cover 1 upper surface is vertically installed with screw rod 22, and the screw on the pivoted arm 21 is set on the screw rod 22 and threaded engagement with it.When needs are closed the opening of upper cover 15, pivoted arm 21 is turned to second place place, this moment kettle cover 1 just be positioned at upper cover 15 upper end open directly over, handwheel, handle, spanner etc. are provided in screw rod 22 upper ends, and drive screw 22 rotates and kettle cover 1 is pressed down with upper cover 15 flanges fit tightly, can finish the sealing assembling of kettle cover 1.And the mode of opening kettle cover 1 is just opposite with above-mentioned steps.In addition, also be provided with gas phase mouth 16 on the tube wall of upper cover 15, be used for the cut of output gas phase and be delivered to condenser by tube connector 17.
Described evaporimeter comprises along the tubulose heating jacket 7 of described inner wall of kettle continuous distributed and the coaxial heating tube 11 that is arranged in the described kettle, described heating tube 11 and the heating jacket 7 interior heating chambers 10 that only circulate for conduction oil that form respectively mutually isolation, each heating chamber 10 is in communication with the outside by oil inlet pipe and flowline respectively.Participate in shown in Figure 2ly, it is outer that heating tube 11 is communicated to kettle by oil inlet pipe a2 and flowline a3, and oil inlet pipe a2 and flowline a3 seal successively passes through heating jacket 7 and inner wall of kettle extends to outside the kettle, and can be communicated with heat-conducting oil heating system.It is outer that heating jacket 7 is communicated to kettle by oil inlet pipe a1 and flowline a4, and oil inlet pipe a1 and flowline a4 pass through inner wall of kettle and extend to outside the kettle, and can be communicated with heat-conducting oil heating system.And the zone between described heating tube 11 and heating jacket 7 consists of the heating clamber 12 that is communicated with described vaporization chamber 14, mud chamber 8.
For guaranteeing that forming suitable space (being heating clamber 12) between heating tube and the heating jacket 7 adds thermal material, and make this heating clamber 12 have suitable circulation and turbulent flow, to guarantee the even and less scaling of heating, those heating tubes and heating jacket 7 have following characteristic:
The oil-in of described oil inlet pipe a1, a2 all is positioned at the bottom of described heating chamber 10 inwalls, and the oil-out of described flowline a3, a4 is positioned at the top of described heating chamber 10 inwalls.And in each heating chamber 10, on the inwall that the oil-in in it and oil-out are respectively formed at its both sides.
In addition, the external diameter of described heating tube 11 should be the 15-30% of described kettle internal diameter.
The internal diameter of described heating jacket 7 should be the 65-80% of described kettle internal diameter.
Demister 2 is arranged in the upper cover 15 and is positioned at the below of described gas phase mouth 16, and described demister 2 comprises three networking sheet groups (only for schematically expression, not embodying three networking sheet group structures among the figure).
Shown in Fig. 4-5, described net sheet group is by a plurality of stacked ripple net sheets 20 with crest and trough and hold the housing 19 of fixing those ripple net sheets 20 and consist of successively from top to bottom.In the described net sheet group, should have 60 ° to 120 ° angle between the crest bearing of trend of any two adjacent corrugations net sheets 20.Preferably, the angle that has 90 ° or 75 ° between the crest bearing of trend of any two adjacent corrugations net sheets 20.The section of described ripple net sheet 20 is sine curve shape (referring to Fig. 6) or polyline shaped.Shown in 5, the pitch of waves D of described ripple net sheet 20 should be 3 to 6 times of its peak height h.
Three networking sheet groups from top to bottom overlapping arrangement and have each other the interval.Net sheet group is that horizontally disposed leg 13 fixes on the inwall by described upper cover 15 tube walls, and the outer rim of net sheet group supports by described leg 13, and is for convenience detach to carry out maintenance of clean-up for demister 2 with this.
The erosion control materials device consists of by being located at anti-overflow ring 4 and anti-overflow hat 3 in the kettle, that be positioned at described evaporimeter top.Wherein, described anti-overflow ring 4 is the annulus that arranges continuously on the described inner wall of kettle, wherein is formed centrally communication port 5, and specifically, anti-overflow ring 4 distributes along described still top and kettle body intersection.Anti-overflow hat 3 is fixedly installed between the roof on described anti-overflow ring 4 and still top, and distinguishes separately with the two.Anti-overflow hat 3 is the oval calotte shape with the coaxial setting of described kettle, and parallel with described still top inwall.
For playing good erosion control material effect, have following specific requirement for the structure of anti-overflow ring 4 and anti-overflow hat 3:
The bore of described communication port is the 0.3-0.5 of described kettle internal diameter.
The external diameter of described anti-overflow hat 3 outer rims is greater than the bore of described communication port 5.
Form uniform the first gap between the roof on anti-overflow hat 3 upper surfaces and described still top, described anti-overflow hat 3 lower edges are parallel with described anti-overflow ring 4 upper surfaces and form the second gap.The width in described the second gap is 3-10 times of the first gap.In addition, even interval between the outer rim of anti-overflow hat 3 and described inner wall of kettle, and this interval is greater than the first gap.
By such structure, when material in the still seethes with excitement and upwards boils over, the foam face of its rising should be high along inner wall of kettle, umbilicate form, and higher part is suppressed by anti-overflow ring 4, can only enter zone between anti-overflow ring 4 and the anti-overflow hat 3 by communication port 5, afterwards to around diffuse through the first gap between the roof that the second gap enters anti-overflow hat 3 upper surfaces and described still top.In above-mentioned process, owing to having retrained the circulation path of gas-liquid mixture, liquid component is progressively tackled, remaining part is finally ended by demister 2, and the DOPT of gaseous state is discharged by gas phase mouth 16 by demister 2.
Be the control temperature in the kettle, the top of the up-and-down boundary place of corresponding heating clamber 12 and heating clamber 12 offers respectively temperature-measuring port c1, c2, c3 on the sidewall of described kettle body,, detect the temperature of key position in the still by these three temperature-measuring ports.
In addition, on the sidewall of described kettle body in the corresponding vaporization chamber 14 position of nearly overflow ring 4 and nearly heating clamber 12 offer respectively peep hole.Be packaged with observation window 6 on these three peep holes.
By observation window 6 and temperature-measuring port c1, c2, c3, can make people in time grasp state in the still in the external world, in order in time tackle the situations such as temperature fluctuation, liquid level variation.
In addition, the sidewall of kettle body offers manhole in the position of vaporization chamber 14, is packaged with manhole cover on this manhole, cleans heating tube in the still so that the operator enters by this manhole.
Abovely be elaborated for invention intention of the present utility model and embodiment by embodiment; but the utility model one of ordinary skill in the art be appreciated that; the above embodiment of the utility model only is one of preferred embodiment of the present utility model; be the length restriction; here can not all embodiments of particularize; any enforcement that can embody the utility model claim technical scheme is all in protection domain of the present utility model.
It should be noted that; above content is in conjunction with concrete embodiment further detailed description of the utility model; can not assert that the specific embodiment of the present utility model only limits to this; under the guidance of above-described embodiment; those skilled in the art can carry out various improvement and distortion on the basis of above-described embodiment, and these improvement or distortion drop in the protection domain of the present utility model.

Claims (5)

1. evaporimeter that distills the distillation still of DOTP, related distillation still kettle inside has evaporimeter, be positioned at the vaporization chamber of described evaporimeter top and the mud chamber that is positioned at described evaporimeter below, be provided with a upper cover with described kettle internal communication on the described kettle top, offer gas phase mouth on the described upper cover, bottom, described mud chamber is provided with drainage conduit, it is characterized in that: described evaporimeter comprises along the tubulose heating jacket of described inner wall of kettle continuous distributed and the coaxial heating tube that is arranged in the described kettle, form respectively the heating chamber that only circulates for conduction oil of mutually isolation in described heating tube and the heating jacket, each heating chamber is in communication with the outside by oil inlet pipe and flowline respectively, and the zone between described heating tube and heating jacket consists of and described vaporization chamber, the heating clamber that the mud chamber is communicated with.
2. a kind of evaporimeter that distills the distillation still of DOTP according to claim 1, it is characterized in that: the oil-in of described oil inlet pipe is positioned at the bottom of described heating chamber inwall, and the oil-out of described flowline is positioned at the top of described heating chamber inwall.
3. a kind of evaporimeter that distills the distillation still of DOTP according to claim 2, it is characterized in that: described oil-in and described oil-out are respectively formed at the both sides of described heating chamber.
4. the described a kind of evaporimeter that distills the distillation still of DOTP of any one according to claim 1-3, it is characterized in that: the external diameter of described heating tube is the 15-30% of described kettle internal diameter.
5. a kind of evaporimeter that distills the distillation still of DOTP according to claim 4, it is characterized in that: the internal diameter of described heating jacket is the 65-80% of described kettle internal diameter.
CN 201220617681 2012-11-20 2012-11-20 Evaporator of distillation kettle for distilling dioctyl terephthalate (DOTP) Expired - Fee Related CN202892944U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105817049A (en) * 2016-05-26 2016-08-03 安庆盛峰化工股份有限公司 Alcohol-water separating device of dioctyl phthalate production system
CN105817047A (en) * 2016-05-26 2016-08-03 安庆盛峰化工股份有限公司 Diisobutyl phthalate dealcoholization kettle

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105817049A (en) * 2016-05-26 2016-08-03 安庆盛峰化工股份有限公司 Alcohol-water separating device of dioctyl phthalate production system
CN105817047A (en) * 2016-05-26 2016-08-03 安庆盛峰化工股份有限公司 Diisobutyl phthalate dealcoholization kettle

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