CN216125221U - Double trimethylolpropane extraction system - Google Patents

Double trimethylolpropane extraction system Download PDF

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Publication number
CN216125221U
CN216125221U CN202121980443.3U CN202121980443U CN216125221U CN 216125221 U CN216125221 U CN 216125221U CN 202121980443 U CN202121980443 U CN 202121980443U CN 216125221 U CN216125221 U CN 216125221U
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extraction
backwashing
distributor
ditrimethylolpropane
isooctanol
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CN202121980443.3U
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宋爱华
张刚
李腾飞
方小娟
黄修硕
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Hubei Yihua New Mstar Technology Ltd
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Hubei Yihua New Mstar Technology Ltd
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Abstract

The utility model provides a ditrimethylolpropane extraction system which comprises a proportioning tank, an extraction backwashing device, a recovery device, a plate-frame filtering device, a crystallization device, a discharge pump and a connecting pipeline, wherein the proportioning tank is provided with a feed inlet and a feed outlet; the batching tank comprises a stirring and mixing device and a heating and heat-preserving device; the extraction backwashing device is an extraction backwashing tower, and a packing layer and a distributor are arranged in the extraction backwashing tower. According to the utility model, the distributor and the filler layer are additionally arranged in the extraction backwashing device, so that the mixture and the backwashing liquid can be fully mixed, ditrimethylolpropane can enter the water phase from the oil phase, the oil phase and the water phase are separated, the ditrimethylolpropane is fully dissolved into the water phase, the ditrimethylolpropane is further extracted from the water phase, and the extraction efficiency and the yield are improved; in addition, an extraction backwashing device and a recovery device are arranged, the extraction backwashing device separates a water phase from an oil phase, and isooctanol enters the recovery device in an oil phase form to recover the isooctanol in the oil phase, so that the resource waste is reduced, and the pollution to the environment is avoided.

Description

Double trimethylolpropane extraction system
Technical Field
The utility model belongs to the field of fine chemical engineering, and particularly relates to a ditrimethylolpropane extraction system.
Background
Ditrimethylolpropane (DTMP) is an important fine chemical product, has strong hygroscopicity and strong dissolving capacity on polar substances. Ditrimethylolpropane is a dimer of Trihydroxymethylpropane (TMP) and is also a by-product of the production of trihydroxymethylpropane. The calcium method TMP is a common method for producing TMP, the DTMP content in the byproduct heavy component of the produced TMP can reach about 80 percent, the TMP is used as a base material to extract DTMP, the byproduct is recycled, the resource waste can be reduced, the industrial chain is prolonged, and the method has important significance for increasing the economic benefit of enterprises.
The applicant determines a method for producing DTMP by using TMP recombination as a raw material through a plurality of experiments, and the method specifically comprises the following steps: adding desalted water under the condition of mixing isooctanol and heavy components in a certain proportion for extraction and layering, and separating and crystallizing the water phase to obtain the compound. Based on this, it is necessary to provide a complete set of equipment for producing DTMP by using TMP recombinant as raw material.
SUMMERY OF THE UTILITY MODEL
The utility model provides a ditrimethylolpropane extraction system, which can improve the yield of DTMP and recover isooctyl alcohol, thereby avoiding waste and environmental pollution.
In order to achieve the purpose, the utility model adopts the following technical scheme:
the double trimethylolpropane comprises a proportioning tank, wherein an outlet of the proportioning tank is communicated with a second feed inlet on an extraction backwashing device, an overflow port at the top of the extraction backwashing device is communicated with a recovery device, a discharge port at the bottom of the extraction backwashing device is communicated with an evaporation concentration device, a discharge port at the bottom of the evaporation concentration device is communicated with a filtration device, and the filtration device is communicated with a crystallization device;
the batching tank comprises a stirring and mixing device and a heating and heat-preserving device;
and a packing layer and a distributor are arranged in the extraction backwashing device.
Preferably, the top end of the extraction backwashing device is provided with a first feed inlet, the first feed inlet is connected with a first distributor, the second feed inlet is connected with a second distributor, and the first distributor and the second distributor are arranged oppositely.
Preferably, the packing layers include a top packing layer, an intermediate packing layer, and a bottom packing layer, and the first and second distributors are located between the top packing layer and the intermediate packing layer.
Preferably, the first distributor and the second distributor are uniformly provided with distribution pipes and distribution holes.
Preferably, the bottom of the evaporation concentration device is provided with a concentrated solution discharge port for the solution discharge after the evaporation concentration, recovery unit is isooctanol recovery tower, isooctanol recovery tower top is provided with retrieves the discharge port, is suitable for and retrieves isooctanol in the solution, isooctanol recovery tower bottom is provided with the waste liquid export, is suitable for the waste liquid discharge after retrieving isooctanol.
Preferably, the filter device is a plate and frame filter, the plate and frame filter comprises filter plates and filter frames, and the filter plates and the filter frames are overlapped alternately.
Preferably, the crystallization device comprises a crystallization tank and a temperature control device, wherein the temperature control device is suitable for controlling the temperature in the crystallization tank.
Preferably, discharge pumps, namely a discharge pump, a water phase discharge pump, an oil phase discharge pump and a crystal liquid discharge pump, are arranged between the proportioning tank and the extraction backwashing device, between the extraction backwashing device and the evaporation concentration device, between the extraction backwashing device and the recovery device, and between the evaporation concentration device and the filtering device. Compared with the prior art, the utility model has the beneficial effects that:
(1) (ii) a The method can fully mix the mixture and the backwash liquid, can enable the ditrimethylolpropane to better enter a water phase from an oil phase, separate the oil phase from the water phase, and extract the ditrimethylolpropane from the water phase, and the yield can be as high as 4.3 percent;
(2) according to the utility model, the extraction backwashing device and the recovery device are arranged, the extraction backwashing device separates the oil phase from the water phase, and the isooctanol enters the recovery device in the form of the oil phase to recover the isooctanol in the oil phase, so that the resource waste is reduced, and the environmental pollution is avoided.
Drawings
FIG. 1 is a schematic diagram of a ditrimethylolpropane extraction system provided by an embodiment of the utility model;
FIG. 2 is a cross-sectional view of an extraction backwash tower provided in accordance with an embodiment of the present invention;
FIG. 3 is a schematic diagram of a distributor according to an embodiment of the present invention;
in the drawings, the components represented by the respective reference numerals are listed below:
1. a batching tank; 2. a discharge pump; 3. an extraction backwashing tower; 31. a first feed port; 32. a second feed port; 33. a first distributor; 34. a second distributor; 341. a distribution pipe; 342. a distribution hole; 35. a discharge port; 36. an overflow port; 4. a water phase discharging pump; 5. an oil phase discharge pump; 6. An evaporation concentration device; 7. a recovery device; 8. a discharge pump for the crystallized liquid; 9. a filtration device; 10. A crystallizing device.
Detailed Description
The present invention is further described in detail below with reference to specific examples so that those skilled in the art can more clearly understand the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the utility model described herein are capable of operation in sequences other than those illustrated or described herein.
A double trimethylolpropane extraction system comprises a proportioning tank 1, wherein an outlet of the proportioning tank 1 is communicated with a second feed inlet 32 on an extraction backwashing device 3, an overflow port 36 at the top of the extraction backwashing device is communicated with a recovery device 7, a discharge port 35 at the bottom of the extraction backwashing device is communicated with an evaporation concentration device 6, a discharge port at the bottom of the evaporation concentration device 6 is communicated with a filtering device 9, and the filtering device is communicated with a crystallization device 10; the batching tank 1 comprises a stirring and mixing device and a heating and heat-preserving device; a filler layer and a distributor are arranged in the extraction backwashing device 3. At the batching in-process, add heavy component in proportioning bins 1, isooctanol and desalinized water, stirring misce bene, the mixture gets into in extraction backwash device 3, be provided with the distributor in extraction backwash device 3, can distribute mixing material and backwash liquid respectively, it is more even to make backwash liquid and mixing material distribute, the contact is more abundant, the setting up of packing layer can increase the contact time of backwash liquid and mixing material, make more entering water phase of two trimethylolpropane, be favorable to improving two trimethylolpropane's yield. The solution after extraction and backwashing can form two parts of an oil phase and a water phase, wherein the oil phase part mainly contains isooctanol, dissolves oil phase substances in a mixed material and can be directly used for recovering the isooctanol, the water phase part on the one hand recovers a small part of the isooctanol dissolved in the water phase, on the other hand concentrates the water phase material and is used for extracting the ditrimethylolpropane, the isooctanol existing in the oil phase and the water phase can be effectively recovered and utilized, the resource waste is reduced, and the environmental pollution is avoided.
In order to better separate the oil phase from the water phase, the oil phase ditrimethylolpropane is led into the water phase, the top end of the extraction backwashing device 3 is provided with a first feed inlet 31, the first feed inlet 31 is connected with a first distributor 33, a second feed inlet 32 is connected with a second distributor 34, and the first distributor 33 is arranged opposite to the second distributor 34. The setting of distributor can make the better distribution of mixture and backwash liquid in extraction backwash device 3, thereby avoids solution to concentrate on the contact and the extraction of influence material in less region, and first distributor 33 and second distributor 34 set up relatively, can increase the contact time of mixture and backwash liquid, and that makes among the mixture two trimethylolpropane can be better dissolves to aqueous phase.
The packing layer in the extraction backwashing device 3 comprises a top packing layer, a middle packing layer and a bottom packing layer, the first distributor 33 and the second distributor 34 are both positioned between the top packing layer and the middle packing layer, and the first distributor 33 and the second distributor 34 are uniformly provided with distribution pipes 341 and distribution holes 342. Set up the evenly distributed of realization mixed material and backwash liquid that distribution pipe 341 and distribution hole 342 can be better on the distributor, first distributor 33 and second distributor 34 are located between top packing layer and the middle packing layer, and mixed material and backwash liquid distribute back in extraction backwash device 3 through two distributors respectively, under the effect of packing layer, both stay a period after mixing to mix once more in the packing layer, help the two trimethylolpropane of oil phase to get into in the aqueous phase. The filler layer can be one of grid filler, corrugated filler, pulse filler, tetrafluoro filler and lamination filler.
And the aqueous phase solution containing the ditrimethylolpropane enters an evaporation concentration device 6, and a concentrated solution discharge port is arranged at the bottom of the evaporation concentration device and used for discharging the solution after evaporation concentration. In the evaporation concentration device 6, the aqueous phase solution is concentrated by evaporating redundant water, which is beneficial to improving the ditrimethylolpropane and is convenient for crystallization and precipitation from the aqueous phase solution.
In oil phase solution got into recovery unit 7, recovery unit 7 was isooctanol recovery tower, and isooctanol recovery tower top was provided with retrieves the discharge gate, is suitable for to retrieve isooctanol in the solution, and isooctanol recovery tower bottom is provided with the waste liquid export, is suitable for the waste liquid discharge after retrieving isooctanol. Recovery unit retrieves isooctanol through evaporation condensation, reduces the wasting of resources and to the pollution of environment, and the waste liquid after retrieving is discharged through below waste liquid outlet to carry out innocent treatment.
The extraction system is provided with a filter device 9, the filter device 9 is a plate and frame filter, the plate and frame filter comprises filter plates and filter frames, and the filter plates and the filter frames are overlapped alternately. The concentrated water phase material enters a plate frame filtering device 9, the filter plates and the filter frames are inwards squeezed, filter residues stay between the two filter plates and the filter frames, filtrate flows out of the plate frame, impurities in concentrated solution are removed, and activated carbon can be added into the device to decolor the filtrate.
In order to obtain ditrimethylolpropane, a crystallization device 10 is provided, comprising a crystallization tank and a temperature control device, which is adapted to control the temperature inside said crystallization tank. And (3) enabling the filtrate to enter a crystallization tank, and controlling the temperature of the crystallization tank to be in a proper range through a temperature control device, so that ditrimethylolpropane can be crystallized and separated out from the filtrate, and ditrimethylolpropane is obtained.
In order to better realize the transmission of materials among all devices in the system, discharge pumps, namely a discharge pump 2, a water phase discharge pump 4, an oil phase discharge pump 5 and a crystal liquid discharge pump 8, are arranged between the proportioning tank 1 and the extraction backwashing device 3, between the extraction backwashing device 3 and the evaporation concentration device 6, between the extraction backwashing device 3 and the recovery device 7 and between the evaporation concentration device and the filtering device 9.
When the extraction system is used for extracting ditrimethylolpropane from trimethylolpropane heavy components, the trimethylolpropane heavy components and isooctanol are put into a proportioning tank 1 according to the proportion of 1:1, the temperature of the proportioning tank 1 is controlled to be 85 ℃, the materials are fully stirred and mixed, then desalted water with the volume being 1.5-1.7 times that of the mixed materials is added, the temperature is kept at 80-90 ℃, and the materials are stirred for 2-3 hours, so that the oil phase ditrimethylolpropane can be fully dissolved into a water phase. The prepared materials are input into an extraction backwashing device 3 through a discharge pump 2 and a second feed inlet 32, and are uniformly distributed in an extraction backwashing tower 3 through a distributor 34 connected with the second feed inlet 32, desalted water enters from a first feed inlet 31 at the top end of the extraction backwashing tower 3 and is uniformly distributed in the extraction backwashing tower 3 through a distributor 33, the distributor 33 and the distributor 34 are oppositely arranged, a distribution pipe 341 and distribution holes 342 are uniformly arranged on the distributor, the desalted water and the mixed materials can be fully contacted and mixed, the mixed solution is temporarily stopped and continuously mixed under the action of an intermediate packing layer, and the ditrimethylolpropane in the oil phase is dissolved into the water phase again. The oil phase flows out from an overflow port 36 at the top, is input into a recovery device 7 under the action of an oil phase discharge pump 5, and is subjected to the recovery of isooctanol through the action of evaporation and condensation; the water phase is output from a discharge port 35 at the bottom, and is conveyed into an evaporation concentration device 6 under the action of a water phase discharge pump 4, and the water phase material is concentrated in the evaporation concentration device 6, so that the concentration of the ditrimethylolpropane in the water phase is further improved. The concentrated water phase material enters a filtering device 9, the filtering device 9 is a plate and frame filter, active carbon is added into the plate and frame filter, the concentrated water phase material is subjected to filter pressing to remove impurities, and meanwhile, the active carbon can decolor the water phase material. The filtrate was introduced into a crystallizing tank of the crystallizing device 10, and the temperature in the crystallizing tank was controlled at 16 ℃ by a temperature control device to crystallize and precipitate ditrimethylolpropane from the solution.
Specifically, the procedure and the extraction conditions for extracting ditrimethylolpropane using the ditrimethylolpropane extraction system of the present example are as follows:
s1, adding trimethylolpropane heavy components and isooctyl alcohol into a proportioning tank 1 according to the proportion of 1:1, controlling the mixing temperature to be 85 ℃, and fully stirring and mixing for 1-2 h;
s2, adding desalted water with the volume of 1.5-1.7 times that of the mixed material into the batching tank 1, heating to 80-90 ℃, and stirring for 2-3 hours to enable the oil phase ditrimethylolpropane to be fully dissolved into the water phase;
s3, inputting the prepared materials into an extraction backwashing tower 3 through a discharge pump 2, inputting desalted water for backwashing and layering, discharging an oil phase through an overflow port 36 at the top of the extraction backwashing tower 3, and recovering isooctanol through a recovery device 7;
s4, inputting the water-phase material into the evaporation concentration device 6 through a discharge hole 35 at the bottom of the extraction backwashing tower 3 to recover the isooctanol and concentrate the water-phase material, wherein the concentrated water-phase material is a crystal liquid;
s5, inputting the crystallization liquid obtained in the step S4 into a filtering device 9, wherein the filtering device 9 is a plate and frame filter, and active carbon is added to decolor the crystallization liquid while the plate and frame filter carries out filter pressing on the crystallization liquid;
s6, filtering the decolorized crystallization liquid in the step S5, inputting the decolorized crystallization liquid into a crystallization tank of the crystallization device 10, and crystallizing the crystallization liquid by keeping the temperature of the crystallization tank at 16 ℃ to obtain ditrimethylolpropane crystals.
The mechanisms, components and parts of the present invention which are not described in detail are all the existing structures which exist in the prior art. Can be purchased directly from the market.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. The double trimethylolpropane extraction system is characterized by comprising a proportioning tank (1), wherein an outlet of the proportioning tank (1) is communicated with a second feed inlet (32) on an extraction backwashing device (3), an overflow port (36) at the top of the extraction backwashing device (3) is communicated with a recovery device (7), a discharge port (35) at the bottom of the extraction backwashing device (3) is communicated with an evaporation concentration device (6), a discharge port at the bottom of the evaporation concentration device (6) is communicated with a filter device (9), and the filter device (9) is communicated with a crystallization device (10); the batching tank (1) comprises a stirring and mixing device and a heating and heat-preserving device;
a packing layer and a distributor are arranged in the extraction backwashing device (3).
2. The extraction system of ditrimethylolpropane according to claim 1, characterized in that the top end of the extraction backwashing device (3) is provided with a first feed inlet (31), the first feed inlet (31) is connected with a first distributor (33), the second feed inlet (32) is connected with a second distributor (34), and the first distributor (33) and the second distributor (34) are arranged oppositely.
3. The system of claim 2, wherein the packing layers comprise a top packing layer, an intermediate packing layer, and a bottom packing layer, and the first distributor (33) and the second distributor (34) are located between the top packing layer and the intermediate packing layer.
4. The ditrimethylolpropane extraction system according to claim 3, wherein the first distributor (33) and the second distributor (34) are uniformly provided with distribution pipes (341) and distribution holes (342).
5. The extraction system of ditrimethylolpropane according to claim 1, wherein the bottom of the evaporation concentration device (6) is provided with a concentrated solution discharge port for discharging the solution after evaporation concentration, the recovery device (7) is an isooctanol recovery tower, the top of the isooctanol recovery tower is provided with a recovery discharge port suitable for recovering isooctanol in the solution, and the bottom of the isooctanol recovery tower is provided with a waste liquid outlet suitable for discharging the waste liquid after recovery of isooctanol.
6. The ditrimethylolpropane extraction system according to claim 1, wherein the filtering device (9) is a plate and frame filter comprising filter plates and filter frames, the filter plates and the filter frames being alternately stacked.
7. The ditrimethylolpropane extraction system according to claim 1, wherein the crystallization device (10) comprises a crystallization tank and a temperature control device adapted to control the temperature inside the crystallization tank.
8. The extraction system of ditrimethylolpropane according to any one of claims 1-7, wherein discharge pumps are respectively arranged between the proportioning tank (1) and the extraction backwashing device (3), between the extraction backwashing device (3) and the evaporation concentration device (6), between the extraction backwashing device (3) and the recovery device (7), and between the evaporation concentration device (6) and the filtration device (9), and are respectively a discharge pump (2), a water phase discharge pump (4), an oil phase discharge pump (5) and a crystal liquid discharge pump (8).
CN202121980443.3U 2021-08-20 2021-08-20 Double trimethylolpropane extraction system Active CN216125221U (en)

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CN202121980443.3U CN216125221U (en) 2021-08-20 2021-08-20 Double trimethylolpropane extraction system

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