CN111410601A - Method and device for extracting ditrimethylolpropane from trimethylolpropane heavy component - Google Patents
Method and device for extracting ditrimethylolpropane from trimethylolpropane heavy component Download PDFInfo
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- CN111410601A CN111410601A CN202010246777.1A CN202010246777A CN111410601A CN 111410601 A CN111410601 A CN 111410601A CN 202010246777 A CN202010246777 A CN 202010246777A CN 111410601 A CN111410601 A CN 111410601A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/38—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
Abstract
The invention belongs to the technical field of purification and processing of ditrimethylolpropane, and particularly relates to a method for extracting ditrimethylolpropane from trimethylolpropane heavy components, which is characterized by comprising the following steps: step 1, preparing a light phase, wherein the light phase adopts a uniformly stirred mixture of trimethylolpropane heavy component and isooctanol; step 2, selecting a heavy phase, wherein the heavy phase adopts process water; step 3, adding the light phase obtained in the step 1 and the heavy phase obtained in the step 2 into an extraction device for extraction, and separating liquid to obtain an extraction phase and a raffinate phase; step 4, rectifying and separating the extract phase to obtain a distillate component and a kettle liquid; step 5, taking the kettle liquid to cool and crystallize in a crystallization device, wherein the crystallization end point temperature is more than 0 ℃; step 6, centrifugally separating to obtain a crystalline liquid and a solid phase, and washing the solid phase with water until the conductivity of washing water is less than or equal to 200 mu s/cm; step 7, centrifuging the solid phase washed in the step 6 again to obtain a ditrimethylolpropane crude product; step 8, placing the crude ditrimethylolpropane obtained in the step 7 into a vacuum evaporator for dehydration, wherein the absolute pressure of the vacuum evaporator is not more than 2 kPa; and 9, carrying out hot flaking on the crude ditrimethylolpropane product dehydrated in the step 8 to obtain a solid, namely a ditrimethylolpropane product. The method has the advantages that the process does not need high temperature, and organic matters are not decomposed; the product has high content and good chroma; the product extraction rate is high.
Description
Technical Field
The invention belongs to the technical field of purification and processing of ditrimethylolpropane, and particularly relates to a method and a device for extracting ditrimethylolpropane from trimethylolpropane heavy components.
Background
The ditrimethylolpropane is a high value-added chemical and can be used for producing products such as photocuring materials, cosmetics, PVC stabilizers, lubricating oil, defoaming agents, photosensitive materials and the like. Ditrimethylolpropane is generally a byproduct of the trimethylolpropane condensation reaction, concentrated in the trimethylolpropane heavy component. Since the trimethylolpropane heavy component contains a large amount of impurities such as trimethylolpropane cyclic formal, ditrimethylolpropane formal, trimethylolpropane oxetane, colored tar, etc. This makes extraction of ditrimethylolpropane very difficult.
The existing production methods of ditrimethylolpropane mainly comprise two methods:
firstly, a high-temperature rectification-water solvent crystallization method causes further deepening of the color of materials and pyrolysis of organic matters due to high-temperature heating in the production process.
And secondly, the water is used as a solvent for leaching-crystallizing, and other impurities and coloring tar in heavy components are difficult to separate due to water leaching, so that the product content is low and the color difference is low.
The extraction rate of the two conventional processes can only reach 15-30%, the extraction rate is low, and the ditrimethylolpropane with high purity and good chromaticity is difficult to obtain.
In the prior art, a production method which can produce high-content ditrimethylolpropane with good chromaticity, does not need high temperature in the process and does not decompose organic matters is lacked.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method and a device for extracting ditrimethylolpropane from trimethylolpropane heavy components, so as to solve the defects of low extraction rate, poor chromaticity, low purity, high energy consumption of the process, organic matter decomposition and the like of ditrimethylolpropane in the prior art.
The invention discloses a method for extracting ditrimethylolpropane from trimethylolpropane heavy components, which comprises the following steps:
step 1, preparing a light phase, wherein the light phase adopts a trimethylolpropane heavy component and isooctanol mixture which is uniformly stirred.
And 2, selecting a heavy phase, wherein the heavy phase adopts process water.
And 3, adding the light phase obtained in the step 1 and the heavy phase obtained in the step 2 into an extraction device for extraction, and separating liquid to obtain an extraction phase and a raffinate phase.
And 4, rectifying and separating the extract phase to obtain a distillate component and a kettle liquid.
And 5, taking the kettle liquid to cool and crystallize in a crystallization device, wherein the crystallization end point temperature is more than 0 ℃.
And 6, centrifugally separating to obtain mother liquor and a solid phase, and washing the solid phase with water until the conductivity of the washing water is less than or equal to 200 mu s/cm.
And 7, centrifuging the solid phase washed in the step 6 again to obtain a crude product of the ditrimethylolpropane.
And 8, putting the crude ditrimethylolpropane obtained in the step 7 into a vacuum evaporator for dehydration, wherein the absolute pressure of the vacuum evaporator is not more than 2 kPa.
And 9, carrying out hot flaking on the crude ditrimethylolpropane product dehydrated in the step 8 to obtain a solid, namely a ditrimethylolpropane product.
Further, the light phase of step 1, in volume fraction, VTrimethylolpropane heavy component：VIsooctyl alcohol＝1:0.8-1.5。
Furthermore, the process water in the step 2 adopts at least one of pure water, ditrimethylolpropane washing water and ditrimethylolpropane mother liquor.
Further, in step 3, in volume fraction, VLight phase:VHeavy phase＝1:2-6。
Further, the feeding temperature of the light phase and the heavy phase in the step 3 is 50-95 ℃.
Further, the raffinate phase in the step 3 is used for recovering isooctanol.
Further, in the rectification operation in the step 4, the temperature at the top of the tower is 95-98 ℃, and the temperature at the bottom of the kettle is 102-105 ℃.
Further, the distillate components in the step 4 comprise isooctyl alcohol and water, and can be purified and recycled to prepare a light phase.
Preferably, in the trimethylolpropane heavy component described in the step 1, the trimethylolpropane content is not more than 16% and the ditrimethylolpropane content is not less than 30% by mass fraction.
The invention further discloses a device for extracting ditrimethylolpropane from the trimethylolpropane heavy component, which comprises a preparation device, an extraction device, a rectification device, a crystallization separation device, a washing device, a dehydration device and a sheeting device.
The preparation device comprises a light phase preparation tank, an isooctanol storage tank and a heavy component raw material storage tank; the outlet of the isooctanol storage tank is connected with the inlet of the light phase preparation tank, and the outlet of the heavy component raw material storage tank is connected with the inlet of the light phase preparation tank; the light phase preparation tank is provided with a preparation flowmeter, a preparation valve is arranged at the outlet of the light phase preparation tank, the preparation valve is a self-control regulating valve, and the preparation flowmeter is interlocked with the opening of the preparation valve in a self-control mode and used for controlling the liquid outlet flow of the light phase preparation tank.
The extraction device comprises a heavy phase storage tank and a multi-stage extractor; the outlet of the light phase preparation tank is connected with the light phase inlet of the multistage extractor, and the outlet of the heavy phase storage tank is connected with the heavy phase inlet of the multistage extractor; the heavy phase storage tank is provided with a heavy phase flowmeter, a heavy phase valve is arranged at the outlet of the heavy phase storage tank and is a self-control regulating valve, and the heavy phase flowmeter is interlocked with the opening self-control of the heavy phase valve and is used for controlling the liquid outlet flow of the heavy phase storage tank.
The rectifying device adopts a rectifying still, and an extract liquor outlet of the multi-stage extractor is connected with an inlet of the rectifying still.
The crystallization separation device comprises a cooling crystallizer and a centrifuge; and the distillation kettle liquid outlet is connected with the inlet of the cooling crystallizer, and the outlet of the cooling crystallizer is connected with the inlet of the centrifuge.
The washing device comprises a water spraying device and a conductivity tester; the water spraying device is arranged on the upper part of the centrifuge, the conductivity tester is arranged at a liquid phase outlet of the centrifuge, and a switch of the water spraying device is interlocked with the conductivity tester in a self-control way.
The dehydration device comprises a vacuum evaporator, and the solid phase washed by the centrifuge enters the vacuum evaporator for dehydration and then is introduced into the sheeting device.
The sheet forming device adopts a sheet forming machine, and a product is obtained after sheet forming.
Further, the cooling crystallizer comprises a crystallization kettle, a heating device and a cooling device; a thermometer is arranged on the crystallization kettle; the temperature rising device adopts a steam pipeline, and a temperature rising regulating valve is arranged at the inlet of the steam pipeline; the cooling device adopts a cooling water pipeline, and a cooling regulating valve is arranged at the inlet of the cooling water pipeline; the thermometer is respectively interlocked with the heating regulating valve and the cooling regulating valve in an automatic control way.
Further, the crystallization kettle adopts at least one of a coil, a jacket and a coil and jacket.
The invention has the beneficial effects that:
1. the process does not need high temperature, and the organic matter is not decomposed.
2. The product has high content and good chromaticity.
3. The product extraction rate is high.
Drawings
FIG. 1 is a flow chart of the apparatus of the present invention.
FIG. 2 is a process flow diagram of the dispensing apparatus of the present invention.
FIG. 3 is a process flow diagram of the extraction apparatus of the present invention.
FIG. 4 is a process flow diagram of the rectification apparatus of the present invention.
FIG. 5 is a process flow diagram of the crystallization separation device, the washing device, the dehydration device and the sheeting device according to the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for extracting ditrimethylolpropane from trimethylolpropane heavy components comprises the following steps:
step 1, preparing a light phase, wherein the light phase adopts a uniformly stirred mixture of trimethylolpropane heavy component and isooctanol; the trimethylolpropane content in the trimethylolpropane heavy component is 15.8 percent, the ditrimethylolpropane content is 68.6 percent, and other impurities are about 15 percent; in volume fraction, VTrimethylolpropane heavy component：VIsooctyl alcohol＝1:0.9。
And 2, selecting a heavy phase, wherein the heavy phase adopts process water.
Step 4, rectifying and separating the extract phase to obtain a distillate component and a kettle liquid; the distillate components comprise isooctyl alcohol and water; and the solid content of the kettle liquid is over 26 percent in terms of mass fraction.
And 5, taking the kettle liquid to cool and crystallize in a crystallization device, wherein the crystallization end point temperature is more than 0 ℃.
And 6, centrifugally separating to obtain a crystalline liquid and a solid phase, and washing the solid phase with water until the conductivity of the washing water is less than or equal to 200 mu s/cm.
And 7, centrifuging the solid phase washed in the step 6 again to obtain a crude product of the ditrimethylolpropane.
And 8, putting the crude ditrimethylolpropane obtained in the step 7 into a vacuum evaporator for dehydration, wherein the absolute pressure of the vacuum evaporator is not more than 2 kPa.
And 9, carrying out hot flaking on the crude ditrimethylolpropane product dehydrated in the step 8 to obtain a solid, namely a ditrimethylolpropane product.
The parameters of the ditrimethylolpropane product are as follows: the ditrimethylolpropane content is 98.1 percent, the melting chroma (platinum-cobalt color number) is 50 percent, and the recovery rate of the ditrimethylolpropane is 84 percent.
As shown in attached figures 1-5, the invention also discloses a device for extracting ditrimethylolpropane from trimethylolpropane heavy components, which comprises a preparation device 1, an extraction device 2, a rectification device 3, a crystallization separation device 4, a washing device 5, a dehydration device 6 and a sheeting device 7.
The preparation device 1 comprises a light phase preparation tank 11, an isooctanol storage tank 12 and a heavy component raw material storage tank 13; an outlet of the isooctanol storage tank 12 is connected with an inlet of the light phase preparation tank 11, and an outlet of the heavy component raw material storage tank 13 is connected with an inlet of the light phase preparation tank 11; the light phase preparation tank 11 is provided with a preparation flow meter, the outlet of the light phase preparation tank 11 is provided with a preparation valve, the preparation valve is a self-control regulating valve, and the preparation flow meter is interlocked with the opening of the preparation valve in a self-control mode and used for controlling the liquid outlet flow of the light phase preparation tank 11.
The extraction device 2 comprises a heavy phase storage tank 21 and a multi-stage extractor 22; the outlet of the light phase preparation tank 11 is connected with the light phase inlet of the multistage extractor 22, and the outlet of the heavy phase storage tank 21 is connected with the heavy phase inlet of the multistage extractor 22; the heavy phase storage tank 21 is provided with a heavy phase flowmeter, the outlet of the heavy phase storage tank 21 is provided with a heavy phase valve, the heavy phase valve is a self-control regulating valve, and the heavy phase flowmeter is interlocked with the opening self-control of the heavy phase regulating valve and used for controlling the liquid outlet flow of the heavy phase storage tank 21.
The rectifying device 3 adopts a rectifying still 31, and an extract liquid outlet of the multistage extractor 22 is connected with an inlet of the rectifying still 31.
The crystallization separation device 4 comprises a cooling crystallizer 41 and a centrifuge 42; and a kettle liquid outlet of the rectifying kettle 31 is connected with an inlet of the cooling crystallizer 41, and an outlet of the cooling crystallizer 41 is connected with an inlet of the centrifuge 42.
The washing device 5 comprises a water spraying device 51 and a conductivity tester 52; the water spraying device 51 is arranged at the upper part of the centrifuge 42, the conductivity tester 52 is arranged at the liquid phase outlet of the centrifuge 42, and the switch of the water spraying device 51 is interlocked with the conductivity tester 52 in a self-control mode.
The dehydration device 6 includes a vacuum evaporator 61, and the solid phase washed by the centrifuge 42 enters the vacuum evaporator 61 to be dehydrated and then is introduced into the sheeting device 7.
The sheet forming device 7 adopts a sheet forming machine, and a product is obtained after sheet forming.
In this embodiment, the cooling crystallizer 41 includes a crystallization kettle and a temperature reduction device; a thermometer is arranged on the crystallization kettle 41; the cooling device adopts a cooling water pipeline, and a cooling regulating valve is arranged at the inlet of the cooling water pipeline; the thermometer is interlocked with the temperature-reducing regulating valve in a self-control way.
In this embodiment, the crystallization vessel 41 is in the form of at least one of a coil, a jacket, and a coil and jacket.
Examples 2 to 3
Examples 2-3 were the same apparatus and similar procedure as used in example 1, except for the following parameters (table 1):
TABLE 1 product extraction Process parameter Table
The product parameters obtained are shown in the following table (table 2):
TABLE 2 product parameter Table
| Group of | Ditrimethylolpropane content (m/m%) | Melt color (platinum-cobalt color number) | Recovery rate of ditrimethylolpropane (m/m%) |
| Example 2 | 98.3 | 45 | 78 |
| Example 3 | 98.6 | 40 | 52 |
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for extracting ditrimethylolpropane from trimethylolpropane heavy components is characterized by comprising the following steps:
step 1, preparing a light phase, wherein the light phase adopts a trimethylolpropane heavy component and isooctanol mixture which is uniformly stirred.
And 2, selecting a heavy phase, wherein the heavy phase adopts process water.
And 3, adding the light phase obtained in the step 1 and the heavy phase obtained in the step 2 into an extraction device for extraction, and separating liquid to obtain an extraction phase and a raffinate phase.
And 4, rectifying and separating the extract phase to obtain a distillate component and a kettle liquid.
And 5, taking the kettle liquid to cool and crystallize in a crystallization device, wherein the crystallization end point temperature is more than 0 ℃.
And 6, centrifugally separating to obtain mother liquor and a solid phase, and washing the solid phase with water until the conductivity of the washing water is less than or equal to 200 mu s/cm.
And 7, centrifuging the solid phase washed in the step 6 again to obtain a crude product of the ditrimethylolpropane.
And 8, putting the crude ditrimethylolpropane obtained in the step 7 into a vacuum evaporator for dehydration, wherein the absolute pressure of the vacuum evaporator is not more than 2 kPa.
And 9, carrying out hot flaking on the crude ditrimethylolpropane product dehydrated in the step 8 to obtain a solid, namely a ditrimethylolpropane product.
2. The method of claim 1, wherein the light phase of step 1 is volume fraction, Vtrimethylol propaneTrimethylolpropane heavy component：VIsooctyl alcohol＝1:0.8-1.5。
3. The method of claim 1, wherein the process water in step 2 is at least one of pure water, ditrimethylolpropane washing water and ditrimethylolpropane mother liquor.
4. The method of claim 1, wherein in step 3, V is calculated by volume fractionLight phase:VHeavy phase＝1:2-6。
5. The method for extracting ditrimethylolpropane from trimethylolpropane heavy component according to claim 1, wherein the feeding temperature of the light phase and the heavy phase in step 3 is 50-95 ℃.
6. The method as claimed in claim 1, wherein the rectification in step 4 is carried out at a tower top temperature of 95-98 ℃ and a tower bottom temperature of 102-105 ℃.
7. The method for extracting ditrimethylolpropane from a trimethylolpropane heavy component according to any one of claims 1-6, wherein the trimethylolpropane heavy component in the step 1 has a trimethylolpropane content of not more than 16% and a ditrimethylolpropane content of not less than 30% by mass fraction.
8. The device for extracting ditrimethylolpropane from trimethylolpropane heavy components is characterized by comprising a preparation device (1), an extraction device (2), a rectification device (3), a crystallization separation device (4), a washing device (5), a dehydration device (6) and a sheeting device (7).
The preparation device (1) comprises a light phase preparation tank (11), an isooctanol storage tank (12) and a heavy component raw material storage tank (13); the outlet of the isooctanol storage tank (12) is connected with the inlet of the light phase preparation tank (11), and the outlet of the heavy component raw material storage tank (13) is connected with the inlet of the light phase preparation tank (11); the light phase preparation tank (11) is provided with a preparation flowmeter, the outlet of the light phase preparation tank (11) is provided with a preparation valve, the preparation valve is a self-control regulating valve, and the preparation flowmeter is interlocked with the opening of the preparation valve in a self-control mode and used for controlling the liquid outlet flow of the light phase preparation tank (11).
The extraction device (2) comprises a heavy phase storage tank (21) and a multi-stage extractor (22); an outlet of the light phase preparation tank (11) is connected with a light phase inlet of the multistage extractor (22), and an outlet of the heavy phase storage tank (21) is connected with a heavy phase inlet of the multistage extractor (22); the heavy phase storage tank is characterized in that a heavy phase flowmeter is arranged on the heavy phase storage tank (21), a heavy phase valve is arranged at an outlet of the heavy phase storage tank (21), the heavy phase valve is a self-control regulating valve, and the heavy phase flowmeter is interlocked with the self-control of the opening of the heavy phase valve and used for controlling the liquid outlet flow of the heavy phase storage tank (21).
The rectifying device (3) adopts a rectifying still (31), and an extract liquid outlet of the multistage extractor (22) is connected with an inlet of the rectifying still (31).
The crystallization separation device (4) comprises a cooling crystallizer (41) and a centrifuge (42); and a kettle liquid outlet of the rectifying kettle (31) is connected with an inlet of the cooling crystallizer (41), and an outlet of the cooling crystallizer (41) is connected with an inlet of the centrifuge (42).
The washing device (5) comprises a water spraying device (51) and a conductivity tester (52); the water spraying device (51) is arranged at the upper part of the centrifuge (42), the conductivity tester (52) is arranged at a liquid phase outlet of the centrifuge (42), and a switch of the water spraying device (51) is interlocked with the conductivity tester (52) in a self-control mode.
The dehydration device (6) comprises a vacuum evaporator (61), and the solid phase washed by the centrifuge (42) enters the vacuum evaporator (61) for dehydration and then is introduced into the sheeting device (7).
The sheet forming device (7) adopts a sheet forming machine, and a product is obtained after sheet forming.
9. The apparatus for extracting ditrimethylolpropane from trimethylolpropane heavy component according to claim 8, wherein the cooling crystallizer (41) comprises a crystallization kettle (411), a temperature raising device (412), a temperature lowering device (413); a thermometer is arranged on the crystallization kettle (411); the temperature rising device (412) adopts a steam pipeline, and a temperature rising regulating valve is arranged at the inlet of the steam pipeline; the cooling device (413) adopts a cooling water pipeline, and a cooling regulating valve is arranged at the inlet of the cooling water pipeline; the thermometer is respectively interlocked with the heating regulating valve and the cooling regulating valve in an automatic control way.
10. The apparatus for extracting ditrimethylolpropane from trimethylolpropane heavy component according to claim 9, wherein the crystallization kettle (411) is in the form of at least one of a coil, a jacket, a coil plus jacket.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005023067A (en) * | 2003-06-13 | 2005-01-27 | Mitsubishi Gas Chem Co Inc | Method for producing ditrimethylolpropane |
| CN103467252A (en) * | 2013-09-05 | 2013-12-25 | 百川化工(如皋)有限公司 | Method for increasing purity of di-trimethylolpropane |
| CN109485554A (en) * | 2018-11-27 | 2019-03-19 | 濮阳市永安化工有限公司 | The method of double trimethylolpropane is isolated from trimethylolpropane heavy constituent |
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- 2020-03-31 CN CN202010246777.1A patent/CN111410601A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005023067A (en) * | 2003-06-13 | 2005-01-27 | Mitsubishi Gas Chem Co Inc | Method for producing ditrimethylolpropane |
| CN103467252A (en) * | 2013-09-05 | 2013-12-25 | 百川化工(如皋)有限公司 | Method for increasing purity of di-trimethylolpropane |
| CN109485554A (en) * | 2018-11-27 | 2019-03-19 | 濮阳市永安化工有限公司 | The method of double trimethylolpropane is isolated from trimethylolpropane heavy constituent |
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Application publication date: 20200714 |