CN211636466U - Device for preparing electronic-grade propylene glycol monomethyl ether - Google Patents
Device for preparing electronic-grade propylene glycol monomethyl ether Download PDFInfo
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- CN211636466U CN211636466U CN202021867678.7U CN202021867678U CN211636466U CN 211636466 U CN211636466 U CN 211636466U CN 202021867678 U CN202021867678 U CN 202021867678U CN 211636466 U CN211636466 U CN 211636466U
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Abstract
The utility model discloses a preparation electronic grade propylene glycol monomethyl ether's device belongs to fine chemicals apparatus for producing technical field. The device for preparing the electronic-grade propylene glycol monomethyl ether comprises a micro-channel reactor, a dealcoholization tower, a thin film evaporator and a rectifying tower; the microchannel reactor is connected with the dealcoholization tower through a discharge pipeline; the dealcoholization tower is sequentially connected with the thin film evaporator and the rectifying tower through a discharge pipeline of the tower kettle; a circulating pipeline of the dealcoholization tower is connected with the microchannel reactor; the circulating pipeline of the rectifying tower is connected with the dealcoholization tower. The device provided by the utility model, simple process, reaction condition is mild, and the yield is high, and product quality is stable, and can reduce the three wastes and handle.
Description
Technical Field
The utility model relates to a fine chemicals apparatus for producing technical field, concretely relates to preparation electronic grade propylene glycol monomethyl ether's device.
Background
Propylene glycol monomethyl ether (PM) is a solvent with excellent performance and lower toxicity, and has the characteristics of strong dissolving capacity, low volatility, high flash point and the like. The electronic grade propylene glycol monomethyl ether is mainly used for TFT-LCD light resistance thinner, light resistance removing liquid, stripping agent, cleaning agent for IC, light resistance removing buffer, etching agent process and other chemical products needing special specification in the production process of liquid crystal display screen and photoresist. And is widely used as a solvent for producing electronic materials. The molecular structure and the physical and chemical properties of PM are similar to those of glycol ether, and the PM is considered to be an ideal substitute product of the glycol ether with higher toxicity. Propylene glycol monomethyl ether is gradually replacing ethylene glycol monomethyl ether with higher toxicity to become a solvent which is increasingly widely used, the annual demand is gradually increased, and the production, development and utilization prospects are very wide.
The common method for preparing propylene glycol monomethyl ether is Propylene Oxide (PO) method, i.e. PO and lower fatty alcohol react under the catalysis of acid or alkali to prepare the product. At present, the propylene glycol monomethyl ether is prepared by adopting an intermittent kettle type production process in China, and although the method has the advantages of low investment and quick response, the production device has small scale, high material consumption and energy consumption and unstable yield and quality. The developed countries abroad adopt the continuous production process, such as the continuous reaction process of the continuous pressurized reaction process developed by U.S. Shell company, and although the production process has large scale of devices and strong production capacity, the process is complex, and the yield and the selectivity of the propylene glycol ether monoether are not ideal.
SUMMERY OF THE UTILITY MODEL
The utility model discloses to preparation electron level propylene glycol monomethyl ether technology complicacy among the above-mentioned background art, the yield is low, and the unstable technical problem of product quality provides a preparation electron level propylene glycol monomethyl ether's device, simple process, and reaction condition is mild, and the yield is high, and product quality is stable, and can reduce the three wastes and handle.
In order to solve the technical problem, the utility model provides a device for preparing electronic-grade propylene glycol monomethyl ether, which comprises a micro-channel reactor, a dealcoholization tower, a film evaporator and a rectifying tower;
the microchannel reactor is connected with the dealcoholization tower through a discharge pipeline; the dealcoholization tower is sequentially connected with the thin film evaporator and the rectifying tower through a discharge pipeline of the tower kettle;
the circulating pipeline of the dealcoholization tower is connected with the microchannel reactor;
and a circulating pipeline of the rectifying tower is connected with the dealcoholization tower.
Preferably, the system further comprises a first condenser and a second condenser; the first condenser is respectively connected with the dealcoholization tower and the microchannel reactor through a circulating pipeline; and the second condenser is respectively connected with the rectifying tower and the dealcoholization tower through a circulating pipeline.
Preferably, the device also comprises a first reflux tank and a second reflux tank; the first reflux tank is respectively connected with the dealcoholization tower and the first condenser through a circulating pipeline; and the second reflux tank is respectively connected with the rectifying tower and the second condenser through a circulating pipeline.
Preferably, the method further comprises a first reboiler and a second reboiler; the first reboiler is connected with the dealcoholization tower through a discharge pipeline of a dealcoholization tower kettle; the second reboiler is connected with the rectifying tower through a discharge pipeline of the rectifying tower kettle.
Preferably, the system further comprises a raw material preheater which is connected with the microchannel reactor through a discharge pipeline.
Preferably, the system further comprises a raw material mixer, and the raw material mixer is connected with the raw material preheater through a discharge pipeline.
Preferably, the device also comprises a buffer tank, and the buffer tank is connected with the rectifying tower through a side line discharge pipeline of the rectifying tower.
Preferably, the system further comprises a catalyst circulating tank, and the catalyst circulating tank is connected with the thin film evaporator through a discharge pipeline.
Preferably, a conveying pump is respectively arranged on each section of feeding and discharging pipeline and a circulating pipeline which are connected with the microchannel reactor, the dealcoholization tower, the thin film evaporator, the rectifying tower, the first reflux tank, the second reflux tank, the first reboiler, the second reboiler, the raw material preheater and the raw material mixer.
Preferably, the microchannel reactor is a corrugated plate type, single screw type, double screw type or horizontal bar type static mixer.
The utility model discloses compare in prior art and obtained following technological effect:
the utility model has the advantages that the methanol, the propylene oxide and the catalyst react in the microchannel reactor, the high-efficiency mass transfer effect of the microchannel reactor and the sufficient mixing among materials provide guarantee for the reaction of the methanol and the propylene oxide, the reaction time is greatly reduced, the materials are instantly and uniformly mixed in an accurate proportion, the excessive local proportion is avoided, and the generation of byproducts is reduced; meanwhile, reaction heat can be timely led out, the reaction temperature is kept stable, the phenomenon of local overheating is avoided, the generation of byproducts is further reduced, and the yield of target products is improved. And the raw materials are in a laminar flow state in the channel, so that the back mixing phenomenon does not exist, the contact chance of propylene oxide with propylene glycol monomethyl ether and water is effectively avoided, the occurrence of series reaction is reduced, and the generation of secondary ether products is reduced, so that toxic byproducts are reduced, and the selectivity of primary ether is improved.
The utility model discloses after reacting in the microchannel reactor, the reaction liquid that will obtain is refined through dealcoholizing, film evaporation and rectification in proper order, and the rational preparation process result realizes the cyclic utilization of each flow, can not introduce impurity, and material utilization rate is high, and the product purity that obtains is high, and the yield is high. The industrial production of electronic-grade propylene glycol monomethyl ether is realized, the metal ions such as sodium, potassium, calcium, magnesium, lead, zinc, iron and the like in the product are less than 5ppb, the moisture content is less than 20ppm, and the requirements of electronic-grade chemicals are met.
Drawings
Fig. 1 is a schematic structural diagram of a production device provided by the present invention;
FIG. 2 is a schematic view of the connection between the metering pump and the raw material mixer according to the present invention;
wherein: 1-raw material mixer, 2-raw material preheater, 3-microchannel reactor, 4-dealcoholization tower, 5-thin film evaporator, 6-rectifying tower, 7-first condenser, 8-first reflux tank, 9-second condenser, 10-second reflux tank, 11-first reboiler, 12-second reboiler, 13-storage tank, 14-metering pump, 15-buffer tank, 16-third condenser, 17-catalyst circulation tank and 18-metering pump.
Detailed Description
The utility model provides a device for preparing electronic-grade propylene glycol monomethyl ether, which comprises a micro-channel reactor 3, a dealcoholization tower 4, a film evaporator 5 and a rectifying tower 6; the microchannel reactor 3 is connected with the dealcoholization tower 4 through a discharge pipeline; the dealcoholization tower 4 is sequentially connected with a thin film evaporator 5 and a rectifying tower 6 through a discharge pipeline of a tower kettle; a circulating pipeline of the dealcoholization tower 4 is connected with the microchannel reactor 3; the circulating pipeline of the rectifying tower 6 is connected with the dealcoholization tower 4.
During operation, raw materials of methanol, propylene oxide and a catalyst enter the microchannel reactor 3 for reaction, the obtained reaction liquid enters the dealcoholization tower 4 through a discharge pipeline for light component removal, and unreacted methanol and propylene oxide with lighter components return to the microchannel reactor 3 through a circulation pipeline at the top of the dealcoholization tower 4; crude propylene glycol monomethyl ether enters a thin film evaporator 5 through a discharge pipeline of a tower kettle of a dealcoholization tower 4 to be evaporated, steam in the thin film evaporator 5 enters a rectifying tower 6 through the discharge pipeline to be refined, the crude propylene glycol monomethyl ether with lighter components returns to the dealcoholization tower 4 through a circulating pipeline at the tower top of the rectifying tower 6 in the rectifying process, heavy component multi-condensed propylene glycol ether is obtained at the tower kettle of the rectifying tower 6, and electronic grade propylene glycol monomethyl ether is obtained at the lateral line of the rectifying tower 6.
In order to enable the raw materials to react sufficiently, the microchannel reactor 3 is preferably a corrugated plate type, single screw type, double screw type or horizontal bar type static mixer. In the present invention, the material of the microchannel reactor 3 is preferably stainless steel, hastelloy or silicon carbide.
In order to maintain the heat balance in the tower, the present invention preferably further comprises a first condenser 7 and a second condenser 9; the first condenser 7 is respectively connected with the dealcoholization tower 4 and the microchannel reactor 3 through circulating pipelines; the second condenser 9 is respectively connected with the rectifying tower 6 and the dealcoholization tower 4 through circulating pipelines.
In order to perform the backflow, the present invention preferably further comprises a first backflow tank 8 and a second backflow tank 10; the first reflux tank 8 is respectively connected with the dealcoholization tower 4 and the first condenser 7 through circulating pipelines; the second reflux drum 10 is connected with the rectifying tower 6 and the second condenser 9 through circulating pipelines, respectively.
In order to maintain the heat balance in the tower, the present invention preferably further comprises a first reboiler 11 and a second reboiler 12; the first reboiler 11 is connected with the dealcoholization tower 4 through a discharge pipeline of a tower kettle of the dealcoholization tower 4; the second reboiler 12 is connected with the rectifying tower 6 through a discharge pipeline of the tower bottom of the rectifying tower 6.
In order to facilitate the multi-propylene glycol ether obtained by the tower kettle of the rectifying tower 6 to be stored, the utility model discloses the preferred still includes holding vessel 13, holding vessel 13 is connected with the discharge pipeline of the tower kettle of the rectifying tower 6.
In order to shorten the reaction time in the microchannel reactor 3, the utility model discloses in preferably still including raw material pre-heater 2, raw material pre-heater 2 is connected with microchannel reactor 3 through discharge line.
In order to make the reaction fully go on, the utility model discloses in preferably still include raw materials blender 1, raw materials blender 1 is connected with raw materials pre-heater 2 through discharging line.
In order to measure the addition of the raw materials, the utility model discloses well preferred still including measuring pump 18, be connected with raw materials blender 1 through discharging line.
In order to receive electronic grade propylene glycol monomethyl ether, the utility model discloses well preferred still include buffer tank 15, buffer tank 15 is connected with rectifying column 6 through rectifying column 6 side line discharge pipeline.
In order to facilitate cooling of the electronic grade propylene glycol monomethyl ether, the present invention preferably further comprises a third condenser 16, wherein the third condenser 16 is connected with the buffer tank 15 through a discharge pipeline.
In order to facilitate the recovery of the catalyst, the present invention preferably further comprises a catalyst circulation tank 17, wherein the catalyst circulation tank 17 is connected with the thin film evaporator 5 through a discharge pipeline.
In order to facilitate the transportation of the raw materials and the reaction products, the utility model discloses in preferably set up the delivery pump 14 respectively on each section of feeding, discharging pipeline and the circulating pipeline that are connected with microchannel reactor 3, dealcoholization tower 4, film evaporator 5, rectifying column 6, first reflux drum 8, second reflux drum 10, first reboiler 11, second reboiler 12, raw materials preheater 2 and raw materials blender 1.
In order to further illustrate the present invention, the following embodiments are described in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
The epoxypropane, the methanol and the catalyst are respectively injected into a raw material mixer 1 through a metering pump 18, mixed by the raw material mixer 1, enter a raw material preheater 2 to preheat the materials to 50 ℃ and then enter a microchannel reactor 3 for reaction. Transferring the obtained reaction liquid into a dealcoholization tower 4 for light component removal (controlling the vacuum degree of the dealcoholization tower 4 to be less than or equal to 5KPa, the tower top temperature to be 90-120 ℃, the tower bottom temperature to be 130-160 ℃, and the reflux ratio to be 5), condensing unreacted methanol and propylene oxide on the tower top by a first condenser 7, returning the unreacted methanol and propylene oxide into the microchannel reactor 3, and feeding the crude propylene glycol monomethyl ether in the tower bottom material into a film evaporator 5.
And (3) conveying the crude propylene glycol methyl ether from the tower bottom of the dealcoholization tower 4 to the thin film evaporator 5 through a conveying pump 14, controlling the temperature of the thin film evaporator 5 at 110-130 ℃, directly introducing steam into a subsequent rectifying tower 6, and returning the residual liquid in the thin film evaporator 5, which is a solution containing the ionic liquid catalyst, to the synthetic catalyst circulating tank 17.
Steam enters a rectifying tower 6 (the vacuum degree of the rectifying tower 6 is controlled to be less than or equal to 5KPa, the temperature of the top of the tower is controlled to be 110-130 ℃, and the temperature of a tower kettle is controlled to be 140-180 ℃) to carry out negative pressure rectification, a light-component-containing propylene glycol monomethyl ether crude product obtained at the top of the tower returns to a dealcoholization tower 4, the recombination obtained at the bottom of the tower is sent to a storage tank 13, and an electronic-grade propylene glycol monomethyl ether product is extracted at the side line.
The utility model discloses a concrete example is applied to explain the principle and the implementation mode of the utility model, and the explanation of the above example is only used to help understand the method and the core idea of the utility model; meanwhile, for the general technical personnel in the field, according to the idea of the present invention, there are changes in the concrete implementation and the application scope. In summary, the content of the present description should not be construed as a limitation of the present invention.
Claims (10)
1. A device for preparing electronic-grade propylene glycol monomethyl ether is characterized by comprising a micro-channel reactor, a dealcoholization tower, a thin film evaporator and a rectifying tower;
the microchannel reactor is connected with the dealcoholization tower through a discharge pipeline; the dealcoholization tower is sequentially connected with the thin film evaporator and the rectifying tower through a discharge pipeline of the tower kettle;
the circulating pipeline of the dealcoholization tower is connected with the microchannel reactor;
and a circulating pipeline of the rectifying tower is connected with the dealcoholization tower.
2. The apparatus of claim 1, further comprising a first condenser and a second condenser; the first condenser is respectively connected with the dealcoholization tower and the microchannel reactor through a circulating pipeline; and the second condenser is respectively connected with the rectifying tower and the dealcoholization tower through a circulating pipeline.
3. The apparatus of claim 2, further comprising a first reflux drum and a second reflux drum; the first reflux tank is respectively connected with the dealcoholization tower and the first condenser through a circulating pipeline; and the second reflux tank is respectively connected with the rectifying tower and the second condenser through a circulating pipeline.
4. The apparatus of claim 1, further comprising a first reboiler and a second reboiler; the first reboiler is connected with the dealcoholization tower through a discharge pipeline of a dealcoholization tower kettle; the second reboiler is connected with the rectifying tower through a discharge pipeline of the rectifying tower kettle.
5. The apparatus of claim 1, further comprising a feed preheater connected to the microchannel reactor via a discharge line.
6. The apparatus of claim 5, further comprising a feedstock mixer coupled to the feedstock preheater by a discharge line.
7. The apparatus of claim 1, further comprising a buffer tank connected to the rectification column via a rectification column side draw line.
8. The apparatus of claim 1, further comprising a catalyst circulation tank connected to the thin film evaporator by a discharge line.
9. The apparatus according to any one of claims 1 to 8, wherein transfer pumps are respectively provided on the feed and discharge pipelines and the circulation pipelines of each section connected to the microchannel reactor, the dealcoholization tower, the thin film evaporator, the rectification tower, the first reflux tank, the second reflux tank, the first reboiler, the second reboiler, the raw material preheater and the raw material mixer.
10. The apparatus of claim 1, wherein the microchannel reactor is a corrugated plate type, single screw type, double screw type, or cross-bar type static mixer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202021867678.7U CN211636466U (en) | 2020-09-01 | 2020-09-01 | Device for preparing electronic-grade propylene glycol monomethyl ether |
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| CN202021867678.7U CN211636466U (en) | 2020-09-01 | 2020-09-01 | Device for preparing electronic-grade propylene glycol monomethyl ether |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112961128A (en) * | 2021-02-19 | 2021-06-15 | 上海昶法新材料有限公司 | Novel production process device for preparing ASA |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112961128A (en) * | 2021-02-19 | 2021-06-15 | 上海昶法新材料有限公司 | Novel production process device for preparing ASA |
| CN112961128B (en) * | 2021-02-19 | 2023-05-16 | 上海昶法新材料有限公司 | Novel production process device for preparing ASA |
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