CN208482035U - The esterification separator of trioctyl trimellitate (TOTM) - Google Patents

The esterification separator of trioctyl trimellitate (TOTM) Download PDF

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Publication number
CN208482035U
CN208482035U CN201820668135.9U CN201820668135U CN208482035U CN 208482035 U CN208482035 U CN 208482035U CN 201820668135 U CN201820668135 U CN 201820668135U CN 208482035 U CN208482035 U CN 208482035U
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China
Prior art keywords
filler
totm
distributor
vapor
liquid
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CN201820668135.9U
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Chinese (zh)
Inventor
郑铁江
蒋国强
曹圣平
杨伟浩
马俊华
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Jiangsu Hundred Sichuan High Science And Technology New Materials Ltd By Share Ltd
Rugao Ran Chemical Materials Co Ltd
Nantong Hundred Sichuan New Materials Co Ltd
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Jiangsu Hundred Sichuan High Science And Technology New Materials Ltd By Share Ltd
Rugao Ran Chemical Materials Co Ltd
Nantong Hundred Sichuan New Materials Co Ltd
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Abstract

This application provides a kind of esterification separators of trioctyl trimellitate (TOTM), including reaction kettle, vapor-liquid separation tower and condenser, vapor-liquid separating device includes two vapour liquid separators being distributed up and down, first backflow distributor, second backflow distributor and accumulator, two vapour liquid separators include the support plate being horizontally supported in vapor-liquid separation tower and pressing plate, the first filler of filler and the second filler are respectively equipped between support plate and pressing plate, the top of the first filler is arranged in first backflow distributor, the top of the second filler is arranged in second backflow distributor, accumulator is equipped with above first backflow distributor and the second backflow distributor, accumulator center is equipped with overflow ducts;Condenser includes shell side and heat exchanger tube, and heat exchanger tube is arranged in shell side, several baffle plates being set on heat exchanger tube is equipped in shell side, baffle plate is for separating shell side;The concentration that the application is able to maintain water in reaction kettle is in relatively low state, so that reaction positive can carry out, improves reaction transformation efficiency.

Description

The esterification separator of trioctyl trimellitate (TOTM)
Technical field
This application involves a kind of esterification of chemicals production engineering device technique field more particularly to trioctyl trimellitate (TOTM) separation Device.
Background technique
When existing trioctyl trimellitate (TOTM) industrial production, mainly using trimellitic anhydride and octanol by just esterification, esterification And refining methd is produced, octanol during esterification is warming up to 200-220 DEG C, evaporates rear portion as raw material Through in supercooling condenser reflux to kettle, a part of uncooled needs flow back again by with after water stratification, nonetheless octanol Still have and largely steam, a large amount of water of reaction generation is more and more, while incomplete miscellaneous ester is reacted in the heated octanol entrainment steamed Not by separation removal, trimellitic anhydride and octanol will all be inhibited to be esterified the reaction for generating trioctyl trimellitate (TOTM), thus Product color number and content is caused to decline.
Therefore, how to be directed to disadvantage present in the above-mentioned prior art and carry out research and development improvement, actually exerted needed for relevant industry Power research and development target, the application designer in view of this, be think and creation idea, designed then with the experience of many years, pass through In many ways sampling test is inquired into and is studied, and repeatedly amendment improvement, be releasing the application.
Such as application No. is: 201520421013.6 Chinese patent discloses a kind of process tower vapor-liquid separating device, by Tower top cooling system, tower bottom cooling system, heat-conducting oil heating system, process tower composition, wherein process tower include spray sprinkler head, 18 layers of float valve tray, 18 layers of float valve tray are distributed in process tower from bottom to up, and spray sprinkler head is located at the top of process tower, the The upper end of 18 layers of float valve tray, it is characterized in that increasing Pall ring in two layers of 18 layers of float valve tray upper end of process tower;This application In process of production, part ethylene glycol does random motion in Pall ring in the mixed vapour of uplink in process tower, increases it Residence time in float valve tray makes full use of shower water to make its trapping that contacts with each other, and reduces ethylene glycol waste to reach Purpose, but this application increases the reaction producing level of reactant by increasing residence time of the reactant in tower, in this way Production efficiency is reduced instead, further increases production cost.
Summary of the invention
(1) technical problems to be solved
It is at low cost this application provides a kind of structure is simple in view of above-mentioned technical problem, it is able to maintain the dense of water in reaction kettle Degree is in relatively low state, so that reaction positive can carry out, improves the ester of the trioctyl trimellitate (TOTM) of reaction transformation efficiency Change separator.
(2) technical solution
This application provides a kind of esterification separator of trioctyl trimellitate (TOTM), including reaction kettle, vapor-liquid separation tower and Condenser, the vapor-liquid separating device include two vapour liquid separators being distributed up and down, the first backflow distributor, the second reflux distribution Device and accumulator, two vapour liquid separators include the support plate being horizontally supported in the vapor-liquid separation tower and pressing plate, institute It states and is respectively equipped with the first filler of filler and the second filler between support plate and the pressing plate, the first backflow distributor setting exists The top of second filler, first reflux point is arranged in the top of first filler, second backflow distributor The accumulator is equipped with above cloth device and second backflow distributor, the accumulator center is equipped with overflow ducts;
The condenser includes shell side and heat exchanger tube, and the heat exchanger tube is arranged in the shell side, is equipped in the shell side Several baffle plates being set on the heat exchanger tube, the baffle plate is for separating the shell side;
The upper and lower ends of the shell side are respectively equipped with upper perforated plate and lower perforated plate, the lower perforated plate and the vapor-liquid separation tower Top is connected, and the side wall of the shell side is equipped with cooling water inlet and cooling water outlet, the baffle plate setting the cold water into Between mouth and the cooling water outlet;
The vapor-liquid separation tower bottom be equipped with gas feed and liquid outlet, the gas feed by gas phase pipeline with it is described Reaction kettle is connected, and the liquid outlet is connected by liquid pipe with the reaction kettle.
In some embodiments of the present application, it is fixedly connected at the top of the lower perforated plate and the vapor-liquid separation tower, it is described Through-hole is equipped in the middle part of lower perforated plate, the lower perforated plate is connected by the through-hole with the vapor-liquid separation tower.
In some embodiments of the present application, first filler and first backflow distributor are welded to connect, described First backflow distributor is detachable backflow distributor, and first backflow distributor center is equipped with the first hollow pipeline, institute It states the first hollow pipeline and matches connection with the overflow ducts.
In some embodiments of the present application, second filler and second backflow distributor are welded to connect, described Second backflow distributor is detachable backflow distributor, and second backflow distributor center is equipped with the second hollow pipeline.
In some embodiments of the present application, second hollow pipeline matches connection with the overflow ducts.
In some embodiments of the present application, the accumulator is annulus seal pan, and the accumulator passes through link of boards There is tapered cap, the tapered cap is located at the surface of the overflow ducts, for blocking the overflow ducts.
In some embodiments of the present application, leakage fluid dram is equipped with below the accumulator, it can will be cold by connected drainage pipe But water is discharged.
In some embodiments of the present application, it is additionally provided with several small apertures on the vapor-liquid separation tower side wall, it is described small to open Hole can be used for radiating or depressurizing.
In some embodiments of the present application, the condenser overhead is additionally provided with offgas outlet, not for relief condenser Cooling steam.
In some embodiments of the present application, first filler and second filler are metal packing.
(3) beneficial effect
It can be seen from the above technical proposal that the application at least has the advantages that one of them:
(1) the esterification separator of trioctyl trimellitate (TOTM) provided by the present application, using the variation of two media phase, By trioctyl trimellitate (TOTM) produce in be used for octanol, water separation, condensation, layering, purification device combine, while can be into Octanol is enriched with into reaction kettle by one step, and the lower water of boiling point is removed in time from system, and the forward direction for maintaining reaction continues It carries out, further improves reaction conversion ratio, while reducing equipment investment cost;
(2) the esterification separator of trioctyl trimellitate (TOTM) provided by the present application passes through the first backflow distributor of setting Liquid can be dispersed in the first filler and the second filler with the second backflow distributor, ascending air is avoided to change without contact Heat and directly reach in condenser, make top water maintain a higher state;
(3) the esterification separator of trioctyl trimellitate (TOTM) provided by the present application, the baffle plate for separating shell side of setting, So that cooling water flows to form tortuous circuit, there is good heat transfer effect, increase condensation effect;
(4) the esterification separator of trioctyl trimellitate (TOTM) provided by the present application, structure is simple, at low cost, is able to maintain anti- It answers the concentration of water in kettle to be in relatively low state, so that reaction positive can carry out, improves reaction transformation efficiency, be conducive to big rule Mould is promoted.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the esterification separator of the application trioctyl trimellitate (TOTM).
[the application main element symbol description]
1, offgas outlet;2, cooling water outlet;3, condenser;301, upper perforated plate;302, lower perforated plate;4, cooling water inlet;5, by Liquid device;6, leakage fluid dram;701, the first backflow distributor;702, the second backflow distributor;801, the first filler;802, it second fills out Material;9, gas feed;10, liquid outlet;11, small aperture.
Specific embodiment
This application provides a kind of structure is simple, at low cost, the concentration for being able to maintain water in reaction kettle is relatively low State improves reaction transformation efficiency, so that reaction positive can carry out conducive to the esterification of the trioctyl trimellitate (TOTM) of large-scale promotion Separator.
For the purposes, technical schemes and advantages of the application are more clearly understood, below in conjunction with specific embodiment, and reference The application is further described in attached drawing.
In the exemplary embodiment of the application, a kind of esterification separator of trioctyl trimellitate (TOTM) is provided. As shown in Figure 1, the application includes reaction kettle, vapor-liquid separation tower and condenser 3, the vapor-liquid separating device includes being distributed up and down Two vapour liquid separators, the first backflow distributor 701, the second backflow distributor 702 and accumulator 5, two vapour liquid separators are equal Including the support plate being horizontally supported in the vapor-liquid separation tower and pressing plate, it is respectively equipped between the support plate and the pressing plate The upper of first filler 801 is arranged in filler the first filler 801 and the second filler 802, first backflow distributor 701 The top of second filler 802, first backflow distributor 701 and institute is arranged in portion, second backflow distributor 702 It states and is equipped with the accumulator 5 above the second backflow distributor 702,5 center of accumulator is equipped with overflow ducts;
The condenser 3 includes shell side and heat exchanger tube, and the heat exchanger tube is arranged in the shell side, is equipped in the shell side Several baffle plates being set on the heat exchanger tube, the baffle plate is for separating the shell side;
The upper and lower ends of the shell side are respectively equipped with upper perforated plate 301 and lower perforated plate 302, the lower perforated plate 302 and the vapour It is connected at the top of liquid knockout tower, the side wall of the shell side is equipped with cooling water inlet 4 and cooling water outlet 2, the baffle plate setting Between the cooling water inlet 4 and the cooling water outlet 2;
The vapor-liquid separation tower bottom be equipped with gas feed 9 and liquid outlet 10, the gas feed 9 by gas phase pipeline with The reaction kettle is connected, and the liquid outlet 10 is connected by liquid pipe with the reaction kettle;The application utilizes two kinds of Jie The variation of matter phase, by trioctyl trimellitate (TOTM) produce in be used for octanol, water separation, condensation, layering, purification device integrate Together, while further octanol can be enriched with into reaction kettle, the lower water of boiling point is removed in time from system, is maintained The forward direction of reaction persistently carries out, and further improves reaction conversion ratio, while reducing equipment investment cost.
Each component part of the present embodiment is described in detail individually below:
Specifically, baffle plate separates shell side, so that cooling water flows to form tortuous circuit, there is good heat exchange effect Fruit increases condensation effect.
Specifically, in this embodiment of the application, as shown in Figure 1, the lower perforated plate 302 and the vapor-liquid separation tower Top is fixedly connected, and through-hole is equipped in the middle part of the lower perforated plate 302, and the lower perforated plate 302 passes through the through-hole and the vapour-liquid point It is connected from tower, the steam between vapor-liquid separation tower and condenser can be facilitated to circulate upwards, condensate liquid circulates downwards.
Specifically, in this embodiment of the application, as shown in Figure 1, first filler 801 and first reflux point Cloth device 701 is welded to connect, and first backflow distributor 701 is detachable backflow distributor, first backflow distributor 701 centers are equipped with the first hollow pipeline, and first hollow pipeline matches connection with the overflow ducts;The application setting Dismountable first backflow distributor 701 can adjust the first backflow distributor according to the amount and reaction environment of different reactants The quantity of 701 distributor pipes, adaptability are stronger.
Specifically, in this embodiment of the application, as shown in Figure 1, second filler 802 and second reflux point Cloth device 702 is welded to connect, and second backflow distributor 702 is detachable backflow distributor, second backflow distributor 702 centers are equipped with the second hollow pipeline, and second hollow pipeline matches connection with the overflow ducts;The application setting Dismountable second backflow distributor 801 can adjust the second backflow distributor according to the amount and reaction environment of different reactants The quantity of 802 distributor pipes, adaptability are stronger.
Specifically, liquid can be dispersed in the first filler by the first backflow distributor 701 and the second backflow distributor 702 801 and second in filler 802, avoid ascending air from directly being reached in condenser 3 without contact heat-exchanging, tie up the water on top Hold a higher state
Specifically, the accumulator 5 is annulus seal pan in this embodiment of the application, the accumulator 5 passes through muscle Plate is connected with tapered cap, and the tapered cap is located at the surface of the overflow ducts, for blocking the overflow ducts;By setting The guide functions for the tapered cap set enter liquid in accumulator 5, and accumulator 5 is arranged to annulus seal pan and facilitates liquid It extracts out or is discharged from drain pipe.
Specifically, being equipped with leakage fluid dram 6 below the accumulator 5 in this embodiment of the application, connected drainage can be passed through Cooling water is discharged pipe.
Specifically, being additionally provided with several small apertures 11, institute on the vapor-liquid separation tower side wall in this embodiment of the application Stating small aperture 11 can be used for radiating or depressurizing, and improves steam and rises and liquid decline poor efficiency.
Specifically, offgas outlet 1 is additionally provided at the top of the condenser 3 in this embodiment of the application, it is cold for discharging The uncooled steam of condenser 3.
First filler 801 and second filler 802 are metal packing, the first filler 801 and the second filler 802 So that gas phase and liquid phase is come into full contact with mass transfer separation, ensure that octanol concentration is constantly increased with decline liquid stream.
Specific working principle: esterification reaction temperature rise to 210 DEG C -220 DEG C with heating, remains negative in tower body Pressure -95Kpa or so, the gas from reaction kettle enter in tower, which mainly contains octanol steam and water vapour, meanwhile, contain There are other a small amount of esters gases, when gas phase rises through gas-liquid separator, and the liquid come above gas-liquid separator occurs Heat exchange, the predominantly water and octanol of liquid in the liquid, since the boiling point under octanol normal pressure is 184 DEG C, higher than the boiling point of water, Under the action of negative pressure, the boiling point of octanol, which remains unchanged, is higher than the boiling point of water, and therefore, the result of heat exchange makes the part water in liquid again Become steam rising, and the part octanol in tail gas is captured into liquid, by the gas-liquid separation of two groups of gas-liquid separators, So that reach in the gas of the lower section of condenser 3,95% the above are water vapour, only a small amount of octanol steam, gases to continue to rise Into condenser 3, in condenser 3, cooling water is left after passing into baffling from cooling water inlet 4 from cooling water outlet 2, takes away heat Amount, so that the steam in condenser 3 is condensed into liquid, condensed liquid is fallen into flowing down under the guiding role of tapered cap In accumulator 5, can be discharged by leakage fluid dram 6 or extraction section liquid, which is mainly water, octanol content less than 5%, It can remove the water generated in reaction kettle, the size of displacement can be roughly the same with the amount for reacting generation water.The uncooled gas in part Body continues to rise, and can be discharged from offgas outlet 1 and carry out subsequent processing.Condensed liquid is most of in addition to fraction is discharged Again from overflow ducts overflow after the full accumulator 5 of stream, gas-liquid separator progress gas-liquid is entered after returning first-class distributor 701 and is divided From;As liquid trickles downwards, the content of octanol is constantly increased, and is flowed into tower body bottom, is then left from liquid outlet 10, into anti- It answers in kettle.The device utilizes the variation of two kinds of different medium liquid phases, and the lower water of boiling point is removed in time from system, maintains The forward direction of reaction persistently carries out.
So far, attached drawing is had been combined the present embodiment is described in detail.According to above description, those skilled in the art There should be clear understanding to the application.
It should be noted that in attached drawing or specification text, the implementation for not being painted or describing is affiliated technology Form known to a person of ordinary skill in the art, is not described in detail in field.In addition, the above-mentioned definition to each element and method is simultaneously It is not limited only to various specific structures, shape or the mode mentioned in embodiment.
It should also be noted that, can provide the demonstration of the parameter comprising particular value herein, but these parameters are without definite etc. In corresponding value, but analog value can be similar in acceptable error margin or design constraint.The side mentioned in embodiment It is only the direction with reference to attached drawing to term, such as "upper", "lower", "front", "rear", "left", "right" etc., is not used to limit this The protection scope of application.In addition, unless specifically described or the step of must sequentially occur, the sequences of above-mentioned steps there is no restriction in It is listed above, and can change or rearrange according to required design.And above-described embodiment can be based on design and reliability Consider, the collocation that is mixed with each other is used using or with other embodiments mix and match, i.e., the technical characteristic in different embodiments can be with Freely form more embodiments.
Particular embodiments described above has carried out further in detail the purpose of the application, technical scheme and beneficial effects Describe in detail it is bright, it is all it should be understood that be not intended to limit this application the foregoing is merely the specific embodiment of the application Within spirit herein and principle, any modification, equivalent substitution, improvement and etc. done should be included in the guarantor of the application Within the scope of shield.

Claims (10)

1. a kind of esterification separator of trioctyl trimellitate (TOTM), including reaction kettle, vapor-liquid separation tower and condenser (3), special Sign is: the vapor-liquid separating device includes two vapour liquid separators being distributed up and down, the first backflow distributor (701), second time Flow distributor (702) and accumulator (5), two vapour liquid separators include the branch being horizontally supported in the vapor-liquid separation tower Fagging and pressing plate are respectively equipped with the first filler of filler (801) and the second filler (802) between the support plate and the pressing plate, First backflow distributor (701) is arranged in the top of first filler (801), second backflow distributor (702) It is arranged in the top of second filler (802), first backflow distributor (701) and second backflow distributor (702) top is equipped with the accumulator (5), and accumulator (5) center is equipped with overflow ducts;
The condenser (3) includes shell side and heat exchanger tube, and the heat exchanger tube is arranged in the shell side, if being equipped in the shell side The dry baffle plate being set on the heat exchanger tube, the baffle plate is for separating the shell side;
The upper and lower ends of the shell side are respectively equipped with upper perforated plate (301) and lower perforated plate (302), the lower perforated plate (302) with it is described It is connected at the top of vapor-liquid separation tower, the side wall of the shell side is equipped with cooling water inlet (4) and cooling water outlet (2), the baffling Plate is arranged between the cooling water inlet (4) and the cooling water outlet (2);
The vapor-liquid separation tower bottom is equipped with gas feed (9) and liquid outlet (10), and the gas feed (9) passes through gas phase pipeline It is connected with the reaction kettle, the liquid outlet (10) is connected by liquid pipe with the reaction kettle.
2. the esterification separator of trioctyl trimellitate (TOTM) according to claim 1, it is characterised in that: the lower perforated plate (302) it is fixedly connected at the top of the vapor-liquid separation tower, through-hole, the lower perforated plate is equipped in the middle part of the lower perforated plate (302) (302) it is connected by the through-hole with the vapor-liquid separation tower.
3. the esterification separator of trioctyl trimellitate (TOTM) according to claim 1, it is characterised in that: first filler (801) it is welded to connect with first backflow distributor (701), first backflow distributor (701) is detachable reflux Distributor, the first backflow distributor (701) center are equipped with the first hollow pipeline, first hollow pipeline and the overflow Channel matches connection.
4. the esterification separator of trioctyl trimellitate (TOTM) according to claim 1, it is characterised in that: second filler (802) it is welded to connect with second backflow distributor (702), second backflow distributor (702) is detachable reflux Distributor, the second backflow distributor (702) center are equipped with the second hollow pipeline.
5. the esterification separator of trioctyl trimellitate (TOTM) according to claim 4, it is characterised in that: described second is hollow Pipeline matches connection with the overflow ducts.
6. the esterification separator of trioctyl trimellitate (TOTM) according to claim 1, it is characterised in that: the accumulator It (5) is annulus seal pan, the accumulator (5) has tapered cap by link of boards, and the tapered cap is located at the overflow ducts Surface, for blocking the overflow ducts.
7. the esterification separator of trioctyl trimellitate (TOTM) according to claim 6, it is characterised in that: the accumulator (5) lower section is equipped with leakage fluid dram (6), cooling water can be discharged by connected drainage pipe.
8. the esterification separator of trioctyl trimellitate (TOTM) according to claim 1, it is characterised in that: the vapor-liquid separation Several small apertures (11) are additionally provided on tower side wall, the small aperture (11) can be used for radiating or depressurizing.
9. the esterification separator of trioctyl trimellitate (TOTM) according to claim 1, it is characterised in that: the condenser (3) top is additionally provided with offgas outlet (1), is used for relief condenser (3) uncooled steam.
10. the esterification separator of trioctyl trimellitate (TOTM) according to claim 1, it is characterised in that: described first fills out Expect (801) and second filler (802) is metal packing.
CN201820668135.9U 2018-05-04 2018-05-04 The esterification separator of trioctyl trimellitate (TOTM) Active CN208482035U (en)

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108392848A (en) * 2018-05-04 2018-08-14 南通百川新材料有限公司 The esterification separator of trioctyl trimellitate (TOTM)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108392848A (en) * 2018-05-04 2018-08-14 南通百川新材料有限公司 The esterification separator of trioctyl trimellitate (TOTM)

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