CN210595865U - Epichlorohydrin's separator - Google Patents
Epichlorohydrin's separator Download PDFInfo
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- CN210595865U CN210595865U CN201921444562.XU CN201921444562U CN210595865U CN 210595865 U CN210595865 U CN 210595865U CN 201921444562 U CN201921444562 U CN 201921444562U CN 210595865 U CN210595865 U CN 210595865U
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Abstract
The utility model discloses a separator of epichlorohydrin specifically is: the device comprises a first rectifying tower, a separating tank, a second rectifying tower, a third rectifying tower, a decanter, a fifth rectifying tower and a sixth rectifying tower, wherein the top of the first rectifying tower is communicated with the separating tank, and the second rectifying tower is communicated in sequence; the bottom of the first rectifying tower is communicated with the third rectifying tower, the decanter, the fifth rectifying tower and the sixth rectifying tower in sequence. The utility model discloses the device has effectively avoided epichlorohydrin to take place to hydrolyze, and the yield is high, and green economy can reduce energy consumption effectively, is fit for extensive industrialization and uses.
Description
Technical Field
The utility model belongs to the technical field of chemical substance separation and purification, especially, relate to a separator of epichlorohydrin.
Background
Epichlorohydrin (ECH), also known as epichlorohydrin, is a colorless liquid, is insoluble in water, is a large organic chemical raw material and a fine chemical product, is a third macrocyclic oxide with the yield inferior to that of ethylene oxide and propylene oxide, is widely applied to the fields of epoxy resin production, glycerin synthesis, epichlorohydrin rubber and the like, can also be used for preparing other derivatives, can also be used as a solvent, a plasticizer, a flame retardant, a surfactant and the like, and is an important organic chemical raw material and an important intermediate of petrochemical industry.
At present, the epichlorohydrin industrial production method in the world mainly comprises 3 methods of propylene high-temperature chlorination method, propylene acetate method and glycerol chlorination saponification method. Among them, the propylene high-temperature chlorination method is the most important production method at home and abroad. At present, the propylene high-temperature chlorination method using propylene as a raw material accounts for about 90% of the total yield, the glycerin chlorination saponification method accounts for 10% of the total yield, and the propylene acetate method is basically eliminated. The propylene high-temperature chlorination method has the technical advantages of flexible production and mature process, but has low yield, high energy consumption, serious equipment corrosion and large discharge of three wastes.
In order to solve the technical defects of the propylene high-temperature chlorination method, US4833260 discloses a method for directly epoxidizing olefin to produce epoxide by using a titanium silicalite molecular sieve as a catalyst and hydrogen peroxide as an oxidant for the first time. The method has mild reaction conditions, is green and environment-friendly, and only water is a byproduct. However, the reaction system adopts methanol as a solvent, and a large amount of circulating solvent exists in the subsequent process, so that the energy consumption for separating the product is high. Meanwhile, an extraction process is adopted in product separation, and the energy consumption for recovering the extractant is also high. In addition, since the reaction product contains water, the separation temperature is too high to cause hydrolysis of epichlorohydrin, further reducing the yield of the objective product. Therefore, reducing the energy consumption for solvent recovery and solving the problem of epichlorohydrin hydrolysis are the key to the large-scale application of the technical process for producing epichlorohydrin by the hydrogen peroxide oxidation method.
Patent CN1534030A discloses a method for separating epichlorohydrin by direct distillation, which is technically characterized in that the distillation is directly carried out in a distillation tower according to the boiling point of the components to separate epichlorohydrin. The process requires a distillation column with a high number of plates and a high reflux ratio to separate the epichlorohydrin. The distillation separation equipment has high investment and large energy consumption. And the epichlorohydrin is subjected to hydrolysis reaction in the distillation process due to the higher distillation temperature, so that byproducts such as chloropropanediol monomethyl ether and chloropropanediol are generated, and the yield of the epichlorohydrin is reduced.
Patent US6350888B1 discloses a process for the separation of epichlorohydrin by means of an extractant, which is technically characterized in that epichlorohydrin is extracted by adding an extractant which is miscible with the reaction liquid, and epichlorohydrin is separated off by distilling off the extractant which is rich in epichlorohydrin. The method requires the use of a large amount of an extractant, and epichlorohydrin and a small amount of methanol are extracted together, so that energy consumption for separating epichlorohydrin and recovering the extractant is extremely high. In addition, the method does not solve the problem of epichlorohydrin hydrolysis during distillation, and the yield of epichlorohydrin is low.
It is worth mentioning that patent CN103420949B discloses an epichlorohydrin separation apparatus, which is technically characterized in that a solution containing epichlorohydrin, methanol, 3-chloropropene and water is mixed with an extractant and then subjected to phase separation to obtain liquid phases rich in epichlorohydrin and methanol, respectively, and the liquid phase rich in epichlorohydrin is distilled to obtain a product. The extractant is an organic solvent which is immiscible with water and contains oxygen atoms and halogen atoms, the capacity of extracting methanol is lower than that of water, the capacity of extracting epichlorohydrin is higher than that of water, and the boiling points of the organic solvent and the epichlorohydrin are different. The process readily achieves phase separation and the product is obtained by distillation of epichlorohydrin. However, a small amount of methanol and water are still extracted together, and the temperature for distilling epichlorohydrin is higher, the energy consumption is greater, and epichlorohydrin is easily hydrolyzed, the method does not fundamentally solve the problem of hydrolysis of epichlorohydrin during distillation, and the yield of epichlorohydrin is still low.
SUMMERY OF THE UTILITY MODEL
In view of this, the utility model aims at providing a epichlorohydrin's separator, overcomes the problem that current epichlorohydrin separator energy consumption is high, epichlorohydrin easily hydrolysises, the yield is low, provides the epichlorohydrin's separator of a low energy consumption to use in large-scale continuous production process. The utility model discloses the device can realize epichlorohydrin separation at low temperature, has effectively avoided epichlorohydrin to take place to hydrolyze, and the yield is high, and green economy can reduce the energy consumption in the disengaging process effectively, and the industrialization using value is big.
In order to achieve the above purpose, the technical scheme of the utility model is realized like this:
the epichlorohydrin separation device comprises a first rectifying tower, a separation tank, a second rectifying tower, a third rectifying tower, a decanter, a fifth rectifying tower and a sixth rectifying tower, wherein the top of the first rectifying tower, the separation tank and the second rectifying tower are communicated in sequence; the bottom of the first rectifying tower, the third rectifying tower, the decanter, the fifth rectifying tower and the sixth rectifying tower are communicated in sequence.
Further, a discharge port at the top of the first rectifying tower is communicated with a feed port of a separation tank, a discharge port at the bottom of the separation tank is communicated with the first rectifying tower, a discharge port at the top of the separation tank is communicated with a feed port of a second rectifying tower, a discharge port at the top of the second rectifying tower is communicated with a reaction system through a pipeline, and a discharge port at the bottom of the second rectifying tower is communicated with the outside;
first rectifying column bottom discharge gate and third rectifying column feed inlet intercommunication, third rectifying column top discharge gate passes through pipeline and reaction system intercommunication, this third rectifying column bottom discharge gate and decanter feed inlet intercommunication, decanter bottom discharge gate and fifth rectifying column feed inlet intercommunication, fifth rectifying column bottom discharge gate and sixth rectifying column feed inlet intercommunication.
And further, the device also comprises a fourth rectifying tower, and a top discharge hole of the decanter and a top discharge hole of the fifth rectifying tower are respectively communicated with a feed inlet of the fourth rectifying tower. The supernatant of the decanter and the light components at the top of the fifth rectifying tower enter a fourth rectifying tower for dehydration, and the waste liquid at the bottom of the tower kettle of the fourth rectifying tower can reach the discharge standard.
Further, the feed inlet of the first rectifying tower is communicated with the reaction system through a pipeline.
Further, the separation device operating conditions are: the temperature is 30-70 ℃, and the pressure is-20 kPa to-90 kPa. Preferably, the separation device is operated at a temperature of 30 deg.C, 35 deg.C, 40 deg.C, 45 deg.C, 50 deg.C, 55 deg.C, 60 deg.C, 65 deg.C or 70 deg.C. Preferably, the operating pressure of the separation device is-20 kPa, -30kPa, -40kPa, -50kPa, -60kPa, -70kPa, -80kPa or-90 kPa.
Further, the separation device operating conditions are: the temperature is 35 ℃, 50 ℃ or 70 ℃, and the pressure is-30 kPa, -50kPa or-70 kPa.
The utility model discloses separator operating condition is mild, at low temperature, goes on under the vacuum state, has avoided epichlorohydrin to take place to hydrolyze, and the product yield is high.
Furthermore, the separation device is used for separating a product obtained after epoxidation reaction of 3-chloropropene and hydrogen peroxide solution by using methanol as a solvent in the presence of a titanium silicalite molecular sieve catalyst. The reaction system is a reaction system which is formed by the epoxidation reaction of 3-chloropropene and hydrogen peroxide solution by taking methanol as a solvent. The reaction product liquid of this reaction is the homogeneous phase, through the utility model discloses a separation process also can reach good separation effect, need not to adopt a large amount of extractants, and the energy consumption is low, has avoided epichlorohydrin to take place to hydrolyze simultaneously, and the product yield is high.
Compared with the prior art, the epichlorohydrin separating device has the following advantages:
(1) the utility model discloses operating condition is mild, at low temperature, goes on under the vacuum state, has avoided epichlorohydrin to take place to hydrolyze, and the product yield is high, and epichlorohydrin product purity is more than 99.9%.
(2) The utility model discloses need not to adopt a large amount of extractants, the process is few, and the energy consumption is low, has further reduced manufacturing cost.
Drawings
The accompanying drawings, which form a part hereof, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without undue limitation. In the drawings:
FIG. 1 is a flow chart of a process for the separation of epichlorohydrin according to an embodiment of the present invention.
Description of reference numerals:
1-a first rectification column; 2-a second rectification column; 3-a third rectifying column; 4-a fourth rectification column; 5-a fifth rectifying tower; 6-a sixth rectifying tower; 7-a separation tank; 8-decanter.
Detailed Description
It should be noted that, in the present invention, the embodiments and features of the embodiments may be combined with each other without conflict.
Example (b):
as shown in fig. 1, the epichlorohydrin separating device comprises a first rectifying tower 1, a separating tank 7, a second rectifying tower 2, a third rectifying tower 3, a decanter 8, a fifth rectifying tower 5 and a sixth rectifying tower 6, wherein the top of the first rectifying tower 1, the separating tank 7 and the second rectifying tower 2 are communicated in sequence; the bottom of the first rectifying tower 1, the third rectifying tower 3, the decanter 8, the fifth rectifying tower 5 and the sixth rectifying tower 6 are communicated in sequence. The feed inlet of the first rectifying tower 1 is communicated with the reaction system through a pipeline.
The top discharge port of the first rectifying tower 1 is communicated with the feed port of the separating tank 7, the bottom discharge port of the separating tank 7 is communicated with the first rectifying tower 1, the top discharge port of the separating tank 7 is communicated with the feed port of the second rectifying tower 2, the top discharge port of the second rectifying tower 2 is communicated with the reaction system through a pipeline, and the bottom discharge port of the second rectifying tower 2 is communicated with the outside. The bottom discharge hole of the first rectifying tower 1 is communicated with the feed inlet of the third rectifying tower 3, the top discharge hole of the third rectifying tower 3 is communicated with the reaction system through a pipeline, the bottom discharge hole of the third rectifying tower 3 is communicated with the feed inlet of the decanter 8, the bottom discharge hole of the decanter 8 is communicated with the feed inlet of the fifth rectifying tower 5, and the bottom discharge hole of the fifth rectifying tower 5 is communicated with the feed inlet of the sixth rectifying tower 6. Still include fourth rectifying column 4, 8 top discharge mouths of decanter, 5 top discharge mouths of fifth rectifying column communicate with 4 feed inlets of fourth rectifying column respectively.
Preferably, the operating conditions of the separation device are that the temperature is 30-70 ℃ and the pressure is-20 kPa-90 kPa. Preferably, the separation device is used for separating a product obtained after epoxidation reaction of 3-chloropropene and hydrogen peroxide solution by using methanol as a solvent in the presence of a titanium silicalite molecular sieve catalyst.
The specific working principle of the epichlorohydrin separation device is as follows:
the epichlorohydrin separation process is carried out at 50 ℃ and under-50 kPa vacuum, and the reaction product liquid comprises 55% of methanol, 23% of chloropropene, 11.3% of epichlorohydrin, 10% of water and the balance of impurities.
Step 1: reaction product liquid from the reaction system enters a first rectifying tower 1, and light components and heavy components are obtained through rectification;
step 2: the light component obtained in the step 1 enters a separation tank 7 for separation, the light component and the heavy component are obtained through separation, and the heavy component returns to the first rectifying tower 1; the separation tank 7 separates out heavy components brought by azeotropy with 3-chloropropene and the like, and the heavy components are returned to the first rectifying tower 1 again;
and step 3: the light component separated by the separation tank 7 in the step 2 enters a second rectifying tower 2, and is further rectified to obtain a light component and a heavy component, the light component with the main component of 3-chloropropene returns to the reaction system, and the heavy component such as chloropropanal polymer and the like is discharged from the second rectifying tower 2 at regular time; 3-chloropropene separated from the top of the second rectifying tower 2 enters a reaction system for recycling, and the purity of the 3-chloropropene is 99.8%;
and 4, step 4: the heavy component obtained in the step 1 enters a third rectifying tower 3, and is further rectified to obtain a light component and a heavy component, and the light component methanol, trace water and epichlorohydrin enter a reaction system for recycling; light components at the top of the third rectifying tower 3 mainly comprise 99.97 percent of methanol, trace water and epichlorohydrin, and the light components enter a reaction system for recycling;
and 5: the heavy component obtained by rectification in the third rectifying tower 3 in the step 4 enters a decanter 8 and is decanted to obtain upper layer liquid and lower layer liquid; the upper layer of the decanter 8 enters a fourth rectifying tower 4, and tower kettle components are used as wastewater for treatment and discharge; the lower layer of the decanter 8 enters a fifth rectifying tower 5 for product pre-separation;
step 6: the lower layer of the decanter 8 lower layer liquid decanter 8 obtained in the step 5 enters a fifth rectifying tower 5, and is further rectified to obtain a light component and a heavy component;
and 7: and (4) the heavy component obtained in the step (6) enters a sixth rectifying tower (6) for further rectification to obtain a light component and a heavy component, wherein the heavy component is treated and discharged, and the light component is an epichlorohydrin product. The epichlorohydrin product is extracted from the top of the sixth rectifying tower 6, the purity is 99.95%, and heavy components in the tower bottom are treated and discharged;
and 8: and (3) feeding supernatant of the decanter 8 obtained in the step (5) and the light component obtained by rectifying the supernatant in the step (6) in the fifth rectifying tower (5) into a fourth rectifying tower (4) for rectifying to obtain a light component and a heavy component, wherein the heavy component in the tower kettle is used as wastewater for treatment and discharge. The supernatant of the decanter 8 and the light components at the top of the fifth rectifying tower 5 enter the fourth rectifying tower 4 for dehydration.
The separation device and the corresponding separation process effectively avoid the hydrolysis of the epichlorohydrin, have high yield, have the purity of the epichlorohydrin product of 99.9 percent, are green and economic, can effectively reduce the energy consumption in the separation process, and are suitable for being applied to large-scale continuous production.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A separation device of epichlorohydrin, comprising a first rectification column (1), a separation tank (7), a second rectification column (2), a third rectification column (3), a decanter (8), a fifth rectification column (5) and a sixth rectification column (6), characterized in that: the top of the first rectifying tower (1), the separating tank (7) and the second rectifying tower (2) are communicated in sequence; the bottom of the first rectifying tower (1), the third rectifying tower (3), the decanter (8), the fifth rectifying tower (5) and the sixth rectifying tower (6) are communicated in sequence.
2. An epichlorohydrin separation apparatus according to claim 1, wherein:
a discharge port at the top of the first rectifying tower (1) is communicated with a feed port of a separation tank (7), a discharge port at the bottom of the separation tank (7) is communicated with the first rectifying tower (1), a discharge port at the top of the separation tank (7) is communicated with a feed port of a second rectifying tower (2), a discharge port at the top of the second rectifying tower (2) is communicated with a reaction system through a pipeline, and a discharge port at the bottom of the second rectifying tower (2) is communicated with the outside;
the device comprises a first rectifying tower (1), a third rectifying tower (3), a decanter (8), a reaction system, a third rectifying tower (3), a third rectifying tower (6), a fifth rectifying tower (5), a third rectifying tower (6), a fourth rectifying tower (6), a fifth rectifying tower (5), a third rectifying tower and a fourth rectifying tower (3).
3. The epichlorohydrin separation apparatus according to claim 1 or 2, wherein: the device is characterized by further comprising a fourth rectifying tower (4), wherein a top discharge hole of the decanter (8) and a top discharge hole of the fifth rectifying tower (5) are respectively communicated with a feed inlet of the fourth rectifying tower (4).
4. The epichlorohydrin separation apparatus according to claim 1 or 2, wherein: the feed inlet of the first rectifying tower (1) is communicated with the reaction system through a pipeline.
5. An epichlorohydrin separation apparatus according to claim 1, wherein: the separation device operating conditions were: the temperature is 30-70 ℃, and the pressure is-20 kPa to-90 kPa.
6. An epichlorohydrin separation apparatus according to claim 1, wherein: the separation device operating conditions were: the temperature is 35 ℃, 50 ℃ or 70 ℃, and the pressure is-30 kPa, -50kPa or-70 kPa.
7. An epichlorohydrin separation apparatus according to claim 1, wherein: the separation device is used for separating a product obtained after epoxidation reaction of 3-chloropropene and hydrogen peroxide solution by using methanol as a solvent in the presence of a titanium-silicon molecular sieve catalyst.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921444562.XU CN210595865U (en) | 2019-09-02 | 2019-09-02 | Epichlorohydrin's separator |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921444562.XU CN210595865U (en) | 2019-09-02 | 2019-09-02 | Epichlorohydrin's separator |
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| CN210595865U true CN210595865U (en) | 2020-05-22 |
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