Equipment with atomizing raw materials continuous production ester class
Technical field
The present invention relates to the used device of organic chemical reactions, more specifically relate to the used equipment of esterification.
Background technology
The synthesizing ester product is mainly realized by esterification; the method of prior art is supplementary material to be heated direct esterification form in reactor; its equipment mainly comprises esterifying kettle and packing tower; esterifying kettle and packing tower communicate; esterification takes place in supplementary material in esterifying kettle; generate the filling surface of moisture in packing tower that the ester time-like produces and form the alternate mass transfer of solution-air two; and obtain refrigerated separation by the refrigerating unit on the packing tower; shut down after reaction is finished, the esters product that takes out in the esterifying kettle carries out different aftertreatments.
There is following problem: a in the production unit of prior art, because esterification is to occur in the esterifying kettle, can only carry out liquid phase reaction, the contact of liquid supplementary material is insufficient, the reaction required time is long; B, supplementary material mix in the disposable adding esterifying kettle in back, have only the supplementary material total overall reaction that adds esterifying kettle to finish after, could shut down the taking-up product; produce then, production process is discontinuous next time, and production efficiency is low; energy loss when causing start to shut down is big, also can lose time.
Summary of the invention
For overcoming the deficiency in the above technology, the invention provides and a kind ofly can shorten reaction time of esterification, and realize the production unit of continuous production esters product.The present invention is achieved through the following technical solutions goal of the invention:
A kind of with the atomize equipment of continuous production ester class of supplementary material, comprise be used to mix, the batching fore-warmer tank (1) of preheating supplementary material, be used to carry supplementary material feed pump (2), be used to carry out degree of depth esterification esterifying kettle (3), be used for the spraying gun (4) of supplementary material atomizing, be used for gaseous substance refrigerative water cooler (5), be used to carry out supplementary material mist attitude esterification inner hollow, be equipped with well heater atomizing esterification column (8), be used for regulating the pressure regulator valve (7) of atomizing esterification column (8) internal pressure; Described batching fore-warmer tank (1) links to each other by pipeline with spraying gun (4), the nozzle of spraying gun (4) stretches into the top in the atomizing esterification column (8), the bottom of atomizing esterification column (8) is connected with esterifying kettle (3) top by pipeline, the top of atomizing esterification column (8) is connected with water cooler (5) by pipeline, pressure regulator valve (7) is installed in the top of water cooler (5), establishes feed pump (2) between batching fore-warmer tank (1) and spraying gun (4).
Principle of work of the present invention is as follows: supplementary material stirs and preheating in batching fore-warmer tank (1), capacity according to atomizing esterification column (8), feed pump (2) pumps to spraying gun (4) with supplementary material and atomizes, send into then in the atomizing esterification column (8), the volume increase of supplementary material atomizing back adds that intensification can make atomizing esterification column (8) internal pressure increase, pressure regulator valve (7) on the water cooler (5) can be opened pressure release at atomizing esterification column (8) when internal pressure is excessive, guarantee device security; The theory reaction flow that is less than or equal to atomizing esterification column (8) when the supplementary material operational throughput of feed pump (2), the amount of esterification column (8) reaction consumes of interior any time that just atomizes is all more than or equal to the operational throughput of feed pump (2), the higher limit that pressure in the atomizing esterification column (8) requires less than the reaction of mist attitude all the time, supplementary material can be carried continuously, be sprayed into atomizing esterification column (8) after the atomizing continuously; Otherwise, if the supplementary material operational throughput of feed pump (2) is greater than the theory reaction flow of atomizing esterification column (8), then the supply of supplementary material is controlled according to the true pressure situation in the atomizing esterification column (8) by feed pump (2), when the lower value of pressure less than mist attitude reaction requirement, atomizing esterification column (8) is sent in feed pump (2) beginning feeding after the supplementary material atomizing; When the higher limit that pressure requires greater than the reaction of mist attitude, the pressure regulator valve (7) on the water cooler (5) is opened pressure release to safety range, and feed pump (2) stops feeding simultaneously; The work in-process that atomizing esterification column (8) lactonization reaction generates flow into esterifying kettle (3) and carry out deep reaction, make finished product through aftertreatment then, the water that esterification generates enters water cooler (5) from atomizing esterification column (8) top and cools off under the effect of band aqua.
For improving the esterification yield of supplementary material, can between atomizing esterification column (8) and esterifying kettle (3), establish filler esterification column (9), the bottom of atomizing esterification column (8) and the top of filler esterification column (9) are connected, and the bottom of filler esterification column (9) and esterifying kettle (3) pass through pipe connection.The liquid form mixt that atomizing esterification column (8) reaction generates enters filler esterification column (9), further reacts under liquid form, has improved the esterification yield of raw material.
Recycle for directly being with aqua, can establish water trap (6) in the below of water cooler (5), the upper end of the lower end of water cooler (5) and water trap (6) is communicated with by pipeline, water trap (6) has band aqua refluxing opening (11) and water port (12), and refluxing opening and spraying gun (4) are communicated with by pipeline.Flow into layering in the water trap (6) through water cooler (5) refrigerative water and band aqua, the band aqua is positioned at the upper strata, and water level is in lower floor, and the epipelagic zone aqua flows back to spraying gun by pipeline and mixes recycling with supplementary material, and lower layer of water is discharged by water port (12).
In order directly liquid catalyst to be recycled, can establish separator (10) before in esterifying kettle (3), separator (10) has inlet (14), liquid catalyst refluxing opening (15) and outlet (16), the inlet of separator (10) is communicated with by pipeline with the bottom of atomizing esterification column (8) or filler esterification column (9), outlet and esterifying kettle (3) are communicated with, and refluxing opening and batching fore-warmer tank (1) are communicated with by pipeline.Liquid mixture that esterification generates and liquid catalyst flow into cooling layering in the separator (10), and liquid mixture flows into esterifying kettle (3) by pipeline and carries out deep reaction, and liquid catalyst flows back to batching fore-warmer tank (1) by pipeline; Also can establish separator (10) afterwards in esterifying kettle (3), the inlet of esterifying kettle (3) and separator (10) is communicated with, and refluxing opening and batching fore-warmer tank (1) are communicated with by pipeline.Liquid mixture that esterification generates and liquid catalyst flow into cooling layering in the separator (10), and liquid mixture enters finishing apparatus after collecting, and liquid catalyst flows back in the batching fore-warmer tank (1) by pipeline, realize the circulation recycling.
Beneficial effect of the present invention
1. spraying gun of the present invention (4) can atomize supplementary material, and atomizing esterification column (8) reacts supplementary material under the state of atomizing, guarantees that supplementary material can fully contact mutually, reacts rapider, shortens the production time greatly.
2. atomize among the present invention esterification column (8) and filler esterification column (9) combined, and makes supplementary material through gaseous state and liquid double reaction, improved conversion of raw material to greatest extent, the quality product of generation and total recovery height.
3. the present invention has adopted water cooler (5), water trap (6) and separator (10), band aqua and liquid catalyst directly reclaims, recycle can have been improved production efficiency.
4. equipment of the present invention can be realized continuous production, and supplementary material can add atomizing esterification column (8) continuously, also can repeatedly add according to the true pressure of when reaction atomizing esterification column (8), product can take out continuously, save the production time greatly, saved energy consumption, reduced cost.
Description of drawings
Fig. 1 is the used device structure synoptic diagram of the embodiment of the invention 1;
Fig. 2 is the used device structure synoptic diagram of the embodiment of the invention 2;
Fig. 3 is the used device structure synoptic diagram of the embodiment of the invention 3;
Fig. 4 is the used device structure synoptic diagram of the embodiment of the invention 4;
Embodiment
Be example to utilize this device fabrication glycerine triacetate below, further specify device structure of the present invention and use-pattern.
Embodiment 1
The present embodiment equipment used comprises batching fore-warmer tank (1), feed pump (2), esterifying kettle (3), spraying gun (4), water cooler (5), atomizing esterification column (8), pressure regulator valve (7) as shown in Figure 1; Described batching fore-warmer tank links to each other by pipeline with spraying gun (4), the nozzle of spraying gun (4) stretches into the top in the atomizing esterification column (8), the top and the water cooler (5) of atomizing esterification column (8) pass through pipe connection, pressure regulator valve (7) is positioned at the upper end of water cooler (5), the bottom of atomizing esterification column (8) is connected with esterifying kettle (3) top by pipeline, establishes feed pump (2) between batching fore-warmer tank (1) and spraying gun (4).
Supplementary material stirs in batching fore-warmer tank (1) and is preheated to 90 ℃, feed pump (2) sprays in the atomizing esterification column (8) after supplementary material is transported to spraying gun (4) atomizing, the heater heats of atomizing esterification column (8) makes temperature rise to 110 ℃, pressure range in the atomizing esterification column (8) is controlled at the 0.6-1.25MPa scope, supplementary material carries out esterification under the mist attitude, the water that esterification generates is under the effect of band aqua, enter water cooler (5) cooling from atomizing esterification column (8) top, the work in-process that esterification generates are sent into esterifying kettle (3) and are carried out deep reaction, carry out aftertreatment then and make finished product.
Embodiment 2
The present embodiment equipment used comprises batching fore-warmer tank (1), feed pump (2), esterifying kettle (3), spraying gun (4), water cooler (5), atomizing esterification column (8), pressure regulator valve (7) and filler esterification column (9) as shown in Figure 2; Described batching fore-warmer tank links to each other by pipeline with spraying gun (4), the nozzle of spraying gun (4) stretches into the top in the atomizing esterification column (8), the top and the water cooler (5) of atomizing esterification column (8) pass through pipe connection, pressure regulator valve (7) is positioned at the top of water cooler (5), be provided with filler esterification column (9) between atomizing esterification column (8) and the esterifying kettle (3), the bottom of atomizing esterification column (8) and the top of filler esterification column (9) are connected, the bottom of filler esterification column (9) and esterifying kettle (3) are communicated with by pipeline, establish feed pump (2) between batching fore-warmer tank (1) and spraying gun (4).
Supplementary material stirs in batching fore-warmer tank (1) and is preheated to 85 ℃, feed pump (2) is transported to spraying gun (4) with supplementary material, spray into after the atomizing in the atomizing esterification column (8), the heater heats of atomizing esterification column (8) makes temperature rise to 105 ℃, pressure range in the atomizing esterification column (8) is controlled at the 0.6-1.25MPa scope, supplementary material carries out esterification, the liquid form mixt that atomizing esterification column (8) reaction generates enters filler esterification column (9), further reaction under liquid form, the water that esterification generates is under the effect of band aqua, enter water cooler (5) cooling from atomizing esterification column (8) top, the work in-process that esterification generates are sent into esterifying kettle (3) and are carried out deep reaction, carry out aftertreatment then and make finished product.
Embodiment 3
The present embodiment equipment used comprises batching fore-warmer tank (1), feed pump (2), esterifying kettle (3), spraying gun (4), water cooler (5), water trap (6), pressure regulator valve (7), atomizing esterification column (8) and filler esterification column (9) as shown in Figure 3; Described batching fore-warmer tank (1) links to each other by pipeline with spraying gun (4), the nozzle of spraying gun (4) stretches into the top in the atomizing esterification column (8), between batching fore-warmer tank (1) and spraying gun (4), establish feed pump (2), be provided with filler esterification column (9) between atomizing esterification column (8) and the esterifying kettle (3), the bottom of atomizing esterification column (8) and the top of filler esterification column (9) are connected, the bottom of filler esterification column (9) and esterifying kettle (3) pass through pipe connection, the top and the water cooler (5) of atomizing esterification column (8) pass through pipe connection, pressure regulator valve (7) is positioned at the upper end of water cooler (5), be provided with water trap (6) in the below of water cooler (5), water trap has inlet on (6), refluxing opening and water port, the inlet of water trap (6) is connected the below of water cooler (5), water port is communicated with extraneous, and refluxing opening is connected to spraying gun (4).
Supplementary material stirs in batching fore-warmer tank (1) and is preheated to 90 ℃, liquid pump (2) is transported to spraying gun (4) with supplementary material, spray into after the atomizing in the atomizing esterification column (8), the heater heats of atomizing esterification column (8) makes temperature rise to 115 ℃, pressure range in the atomizing esterification column (8) is controlled at the 0.6-1.25MPa scope, supplementary material carries out esterification, the liquid form mixt that atomizing esterification column (8) reaction generates enters filler esterification column (9), further reaction under liquid form, the water that esterification generates is under the effect of band aqua, enter water cooler (5) cooling from atomizing esterification column (8) top, the water that esterification generates is under the effect of band aqua, enter water cooler (5) cooling from atomizing esterification column (8) top, the work in-process that esterification generates are sent into esterifying kettle (3) and are carried out deep reaction, carry out aftertreatment then and make finished product.
Embodiment 4
The present embodiment equipment used comprises batching fore-warmer tank (1), feed pump (2), esterifying kettle (3), spraying gun (4), water cooler (5), water trap (6), pressure regulator valve (7), atomizing esterification column (8), filler esterification column (9) and separator (10) as shown in Figure 4; Described batching fore-warmer tank links to each other by pipeline with spraying gun (4), the nozzle of spraying gun (4) stretches into the top in the atomizing esterification column (8), establish feed pump (2) between batching fore-warmer tank (1) and the spraying gun (4), be provided with filler esterification column (9) between atomizing esterification column (8) and the esterifying kettle (3), the bottom of atomizing esterification column (8) and the top of filler esterification column (9) are connected, the bottom of filler esterification column (9) and esterifying kettle (3) pass through pipe connection, be provided with separator (10) between filler esterification column (9) and the esterifying kettle (3), separator (10) has inlet (14), liquid catalyst refluxing opening (15) and outlet (16), the inlet of separator (10) is communicated with by pipeline with the bottom of atomizing esterification column (8) or filler esterification column (9), outlet and esterifying kettle (3) are communicated with, refluxing opening and batching fore-warmer tank (1) are communicated with by pipeline, the top and the water cooler (5) of atomizing esterification column (8) are communicated with by pipeline, pressure regulator valve (7) is positioned at the top of water cooler (5), the below of water cooler (5) is provided with water trap (6), water trap has inlet on (6), refluxing opening and water port, the inlet of water trap (6) is connected the below of water cooler (5), water port is communicated with extraneous, and refluxing opening connects spraying gun (4).
Supplementary material stirs in batching fore-warmer tank (1) and is preheated to 95 ℃, feed pump (2) is transported to spraying gun (4) with supplementary material, spray into after the atomizing in the atomizing esterification column (8), the heater heats of atomizing esterification column (8) makes temperature rise to 100 ℃, pressure range in the atomizing esterification column (8) is controlled at the 0.6-1.25MPa scope, supplementary material carries out esterification, the liquid form mixt that atomizing esterification column (8) reaction generates enters filler esterification column (9), further reaction under liquid form, the water that esterification generates is under the effect of band aqua, enter water cooler (5) cooling from atomizing esterification column (8) top, liquid mixture that esterification generates and liquid catalyst flow into cooling layering in the separator (10), liquid catalyst flows back in the batching fore-warmer tank (1) by pipeline, liquid mixture enters esterifying kettle (3) and carries out deep reaction, carries out aftertreatment then and makes finished product.