CN107098810B - Separation and purification method for preparing electronic-grade propylene glycol monomethyl ether acetate - Google Patents
Separation and purification method for preparing electronic-grade propylene glycol monomethyl ether acetate Download PDFInfo
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- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- C—CHEMISTRY; METALLURGY
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- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention relates to a separation and purification method for preparing electronic-grade propylene glycol monomethyl ether acetate. The original double-tower rectifying device is replaced by a rectifying device with a side line tower in a main separation tower, and a dehydration tower mode is combined to separate and purify a crude product propylene glycol methyl ether acetate containing propylene glycol methyl ether, acetic acid, water and a small amount of heavy components, and metal ions such as Fe contained in the crude product propylene glycol methyl ether acetate are separated and purified by an ion exchange resin bed3+，Na+，K+，Ca2+，Mg2+And the further removal is carried out, so that the electronic grade propylene glycol monomethyl ether acetate product with the acidity less than 80ppm, the water content less than 200ppm and the content of each metal ion less than 1ppb is obtained, and the quality requirement of the current market on electronic chemicals is met. On the premise of not reducing product quality, the method avoids repeated rectification of materials, reduces the investment of tower equipment, reduces the steam consumption of products, and has better economic benefit and environmental benefit by recycling the used ion exchange resin.
Description
Technical Field
The invention relates to a purification method for preparing electronic-grade propylene glycol monomethyl ether acetate, belonging to the field of separation and purification.
Background
Electronic grade propylene glycol methyl ether acetate is a fine chemical with excellent performance, has strong dissolving capacity to polar and non-polar substances due to the fact that the electronic grade propylene glycol methyl ether acetate has three strong chemical function dissolving force factors (groups), namely ether bonds, hydroxyl groups and ester groups, is called as a universal solvent, and is widely used in the industrial fields of coatings, paints, printing, fuels, leather, photosensitive materials, electronic chemicals, high-grade cleaning agents, synthetic brake fluid, jet fuel additives and the like as a solvent or an organic raw material.
As a common electronic chemical, in the modern Integrated Circuit (IC) industry and flat panel display (FDP) industry, electronic grade propylene glycol monomethyl ether acetate is mainly used for preparing a photoresist solvent and a photoresist stripping agent composition, and is sometimes used for cleaning agents of integrated circuits. Along with the intelligent wearing and the rapid development of the panel field, the demand of electronic grade propylene glycol monomethyl ether acetate is more and more large, and the product quality requirement is also continuously improved. The quality index of the electronic grade propylene glycol monomethyl ether acetate comprises the content of metal ions in addition to the boiling range, refractive index, acidity and moisture content required by the conventional industry. At present, some electronic product manufacturers require that the content of various metal ions is less than 5ppb (mu g/kg), some electronic product manufacturers put forward higher requirements, the content of each metal ion is required to be less than 1ppb, and the requirements on the content of the metal ions are higher as the line width of an integrated circuit is narrower and narrower.
Patent CN101993360A discloses a preparation method of electronic grade propylene glycol monomethyl ether acetate, which mainly adopts a strong acid cation exchange resin solid catalyst to replace the original organic acid homogeneous catalyst, so that the residual acid catalyst does not need to be neutralized and removed by adding alkali after the reaction is finished, thereby avoiding the introduction of metal ions in the reaction product due to the addition of inorganic alkali, and simultaneously, the new catalytic system catalyst is easy to separate from the reaction product. In the separation process of subsequent products, cyclohexane or toluene is added into a reaction system as an entrainer of water, and water in the products is removed from the tower top through azeotropic distillation; the dehydrated material enters the next stage of rectification treatment, light fraction at the tower top is unreacted acetic acid and propylene glycol methyl ether, the light fraction returns to a reaction system for recycling, fraction at the tower bottom is common-grade propylene glycol methyl ether acetate, the material passes through a deionization tower, the electronic-grade product propylene glycol methyl ether acetate is arranged at the tower top, heavy components and metal ions to be removed are arranged at the tower bottom, and the content of various metal ions in the electronic-grade product propylene glycol methyl ether acetate prepared by the method is lower than 5 ppb.
Patent CN 202519181U discloses a utility model patent of continuous production electronic level propylene glycol methyl ether acetate device, its main measure also carries out product production optimization through changing the catalysis mode, change original homogeneous phase catalyst into heterogeneous compound solid acid catalyst, change cauldron formula reactor into two-stage fixed bed reactor, the mixed material of esterifying that comes out from the reactor is at first through acetic acid and the propylene glycol methyl ether light component in the lightness-removing tower desorption mixture, the tower cauldron is adopted crude propylene glycol methyl ether acetate and is got into the deionization tower, the top of the tower ejection of compact is electronic level propylene glycol methyl ether acetate, the ejection of compact is the heavy ends raffinate at the bottom of the tower. The product has less than 10ppb of each metal and the patent does not refer to the removal of water from the reaction mixture.
From the disclosures of the above patents, it can be found that the essential contents of the existing patents for preparing electronic grade propylene glycol monomethyl ether acetate are substantially similar, and all the patents are optimized by changing the form of the catalyst, and the original homogeneous reaction is changed into liquid-solid heterogeneous reaction, so that the catalyst and the reaction material can be separated through different phase states, and the neutralization reaction process by adding inorganic base for removing the liquid acid catalyst from the reaction material after the reaction of the homogeneous reaction system is finished is avoided. The step of adding inorganic base is not needed, that is, metal ions are not introduced into a reaction material system, and the electronic grade product with very low metal ion content can be obtained more easily in the subsequent separation process. The rectification mode is generally adopted for removing metal ions.
The invention provides a novel method for separating and purifying a propylene glycol methyl ether acetate crude product, which has the defects of repeated rectification of reaction materials, high product energy consumption and low product purity in the subsequent separation process of a reaction product in the prior patent3+，Na+，K+，Ca2+，Mg2+So as to meet the requirements of electronic-grade products. The method for separating and purifying the crude product can well solve the defects of high production energy consumption and low product purity, and the obtained product has small acidity (calculated by acetic acid)The water content is less than 200ppm, the content of each metal ion is less than 1ppb, and the quality requirement of the existing electronic industry on propylene glycol monomethyl ether acetate products is met.
Disclosure of Invention
The invention provides a separation and purification method of electronic grade propylene glycol monomethyl ether acetate. For the existing propylene glycol methyl ether acetate separation method, the process device mainly adopts a double-tower rectification mode of a light component removal tower and a heavy component removal tower, the whole process is repeatedly rectified, the steam consumption is high, and the reduction of the concentration of metal ions in the product is not facilitated. In order to solve the defects and obtain a product with higher quality, the original rectification mode is replaced by a rectification mode of a main separation tower with a side line tower, and metal ions are further removed from the rectified product through an ion exchange resin bed. The propylene glycol methyl ether acetate product prepared by the method has high purity, meets the requirements of electronic chemical quality, and has acidity of less than 80ppm, water content of less than 200ppm, and content of each metal ion of less than 1 ppb.
The technical scheme of the invention is as follows:
a separation and purification method of electronic grade propylene glycol monomethyl ether acetate comprises the following steps: feeding a propylene glycol methyl ether acetate mixed material containing light components such as water, propylene glycol methyl ether, acetic acid and the like at the outlet of the reactor from the middle part of a dehydration tower, separating the water in the tower through the action of an entrainer, taking out the dehydrated material from a tower kettle, pumping the dehydrated material into the middle part of a propylene glycol methyl ether acetate rectification main tower through a circulating pump, separating light and heavy components, distilling an unreacted raw material mixture of propylene glycol methyl ether, acetic acid and trace water from the tower top, returning the unreacted raw material mixture to the reactor for recycling, feeding a gaseous mixture carrying metal ions and the heavy components into the bottom part of a rectification side line through a connecting pipeline, in the tower, propylene glycol methyl ether acetate migrates upwards, heavy components and metal ions return to the main tower through mass transfer separation and are discharged from the tower bottom, a propylene glycol methyl ether acetate product is collected from the tower top of the side-track tower, and then enters an ion exchange resin bed to further remove the metal ions, and finally an electronic grade propylene glycol methyl ether acetate product with very low metal ion concentration is obtained.
The propylene glycol methyl ether acetate mixed material synthesized by the reactor enters from the middle part of the dehydration tower and is operated under normal pressure. The operating pressure of the dehydration tower is about 0.1MPa, the temperature at the top of the tower is 80-90 ℃, the preference is 88 ℃, and the reflux ratio in the tower is 1.5-3.
The dehydrated mixed material enters from the middle part of the propylene glycol monomethyl ether acetate rectification main tower and is pressurized. The operating pressure of the propylene glycol methyl ether acetate rectification main tower is 0.12-0.2MPa, the tower top temperature is 130-160 ℃, and the reflux ratio of the main tower is 3-8.
The propylene glycol methyl ether acetate and the entrained heavy components enter the side line tower through the connecting pipelines of the main tower and the side line tower, and the pressurization operation is adopted. The operating pressure of the propylene glycol methyl ether acetate rectification side line tower is 0.1-0.18MPa, the tower top temperature is 130-170 ℃, and the tower internal reflux ratio is 0.5-2.
The top of the dehydration tower is provided with an extracted water phase pipeline and is connected with a waste water tank, and the tower kettle is provided with an extracted dehydrated material pipeline and is connected with the middle part of a propylene glycol methyl ether acetate rectification main tower; a side line outlet gas of a stripping section of the propylene glycol methyl ether acetate rectification main tower is connected with a side line tower of the propylene glycol methyl ether acetate rectification by a pipeline; the top of the rectification main tower is provided with a pipeline for extracting light component mixture and returning the light component mixture to the reactor, and the tower kettle is provided with a pipeline for extracting heavy component mixture and connected with a heavy component tank; the top of the rectification side line tower is provided with a pipeline for collecting a propylene glycol methyl ether acetate crude product and is connected with an ion exchange resin bed, and the bottom of the tower is provided with a liquid phase connecting pipeline for returning heavy components to the main tower; the bottom of the ion exchange resin bed is provided with a product pipeline for producing propylene glycol monomethyl ether acetate and is connected with a product tank. A condenser is arranged at the top of the dehydrating tower and connected with a phase splitting tank, an entrainer material pipeline is connected with the phase splitting tank, an extractant reflux pipeline is arranged at the top of an entrainer phase layer, a production pipeline is connected at the bottom of a water phase layer, and a reboiler is arranged at the tower kettle and is heated by steam; arranging a circulating pump at the front end of the dehydrated material pipeline, and pumping the material into the middle part of the rectification main tower; a condenser is arranged at the top of the rectification main tower, part of the light component mixture flows into a production pipeline, and the other part of the light component mixture returns to the top of the tower through a reflux pipeline; a condenser is arranged at the top of the side-line tower, part of the propylene glycol methyl ether acetate crude product flows into a production pipeline, and the other part of the propylene glycol methyl ether acetate crude product returns to the top of the tower through a reflux pipeline; the top of the dehydration tower, the top of the main rectification tower and the top of the side line tower are all cooled by cooling water.
The entrainer is toluene, in the dehydration tower, the toluene and water form a lowest temperature azeotrope, the toluene and water are extracted from the top of the tower and enter a phase separation tank for phase separation, the upper layer of toluene phase returns to the dehydration tower, and the lower layer of water phase is extracted from the bottom.
The dehydration tower, the propylene glycol methyl ether acetate rectification main tower and the side-stream tower adopt a plate tower or a packed tower, and the packed tower is preferred. If the dehydration tower, the rectification main tower and the side line tower are all plate towers, the tower plates adopt float valves or sieve tray plates, and the down-flow area is provided with an overflow weir and a down-flow pipe; if the dehydration tower, the rectification main tower and the side line tower are all packed towers, the packing adopts regular packing, such as plastic regular packing, ceramic regular packing or carbon fiber regular packing, and preferably ceramic corrugated regular packing with the model number of 125Y-700X.
The side line tower is a purifying tower only provided with a rectifying section.
In the ion exchange resin bed, strong acid type cation exchange resin is selected, and preferably macroporous strong acid styrene type cation exchange resin with the model of D001-CC is selected, and as the surface of the ion exchange resin bed has a plurality of voids and large surface area, the ion exchange resin bed has short treatment time and high efficiency when in use; meanwhile, the structure is firm, the repeated transformation expansion rate is low, and the exchange adsorption performance in organic solution is good.
The side line tower and the product storage tank of the main rectification tower of propylene glycol methyl ether acetate adopt stainless steel lining perfluoroalkoxy resin (PFA plastic), so that secondary metal ion pollution in the rectification purification and storage processes can be avoided.
The invention relates to a separation and purification method of electronic grade propylene glycol monomethyl ether acetate, which has the advantages that the original double-tower rectifying device of a light component removal tower and a heavy component removal tower is replaced by a new device which adopts a main rectifying tower and is additionally provided with a side line tower only at a rectifying section at a stripping section, and meanwhile, the mode of combining a dehydrating tower and an ion exchange resin bed is combined, so that the repeated rectification of materials is avoided, the equipment investment of the tower is reduced, and the steam consumption of the product is reduced on the premise of not reducing the product quality. In addition, by the method, the separated materials are effectively reused, the sewage treatment cost is reduced, the electronic grade propylene glycol monomethyl ether acetate product with acidity (calculated by acetic acid) less than 80ppm, water content less than 200ppm and metal ion content less than 1ppb is obtained, the method reduces the investment of tower equipment and the steam consumption of the product, and the used ion exchange resin can be reused by regeneration, thereby saving energy and having better economic benefit and environmental benefit.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 1 shows an illustration:
the device included in the figure comprises a T-1 dehydrating tower, a T-2 propylene glycol methyl ether acetate rectifying main tower, a TS-2 propylene glycol methyl ether acetate rectifying side line tower, a CC ion exchange resin bed, an E-1 dehydrating tower condenser, an E-2 dehydrating tower reboiler, an E-3 propylene glycol methyl ether acetate rectifying main tower condenser, an E-4 propylene glycol methyl ether acetate rectifying main tower reboiler, an E-5 propylene glycol methyl ether acetate rectifying side line tower condenser, a P-1 circulating pump, a V-1 dehydrating tower phase separation tank, a V-2 waste water tank, a V-3 recombination fractional tank and a V-4 electronic grade propylene glycol methyl ether acetate product tank.
The figure also includes the following lines: 1-dehydration tower feed line, 2-entrainer toluene feed line, 3-dehydration tower extractant reflux line, 4-dehydration tower water discharge line, 5-dehydration tower kettle discharge connecting line, 6-propylene glycol methyl ether acetate rectification main tower reflux line, 7-propylene glycol methyl ether acetate rectification main tower top light component extraction line, 8-propylene glycol methyl ether acetate rectification tower kettle heavy component extraction line, 9-rectification main tower and side line tower gas phase connecting line, 10-rectification main tower and side line tower liquid phase connecting line, 11-side line tower reflux line, 12-side tower top product extraction line, 13-electronic grade propylene glycol methyl ether acetate product line.
Detailed Description
The process of fig. 1 represents the advantages of the present invention, but the present invention is not limited to the process of fig. 1, and those skilled in the art can devise various modifications and variations within the technical scope of the inventive concept, and it should be noted that these modifications and variations also fall within the protective scope of the present invention. The invention will be further understood by the following description of the aspects and features of the invention with the aid of the process flow diagram of fig. 1.
The invention is realized by the following technical scheme:
the method for continuously separating and purifying the electronic grade propylene glycol monomethyl ether acetate shown in the attached figure 1 mainly comprises the following steps: the device comprises a dehydration tower, a propylene glycol methyl ether acetate rectification main tower, a propylene glycol methyl ether acetate rectification side line tower, a pump and a pipeline between connecting devices, wherein the top of the dehydration tower and the top of the rectification main tower are provided with condensers, the tower kettle is provided with a reboiler, the top of the side line tower is provided with a condenser, and the tower kettle is connected with the main tower.
The mixture from the synthesis reactor is fed from the middle part of a dehydration tower T-1 through a feed pipeline 1 and is operated under normal pressure, entrainer toluene is introduced from the top of the tower through a pipeline 2 to form a lowest temperature azeotrope with water in the tower, the azeotrope is distilled out from the top of the tower, the mixture is condensed by a condenser E-1 and flows into a phase separation tank V-1 for phase separation, the upper layer toluene phase is taken as the entrainer and returns to the dehydration tower T-1 through a reflux pipeline 3, and the lower layer water phase flows into a waste water tank V-2 through a material pipeline 4 for further treatment. The dehydrated materials are discharged from the tower kettle through a pipeline 5 and are pumped into the middle part of a propylene glycol methyl ether acetate rectification main tower T-2 by a circulating pump P-1 to be pressurized, light components in the tower move upwards, the unreacted raw materials of propylene glycol methyl ether, acetic acid and a trace water mixture are collected from the top of the main tower and are condensed by a condenser E-3 to be divided into two parts, one part returns to the top of the main tower through a backflow pipeline 6, the other part returns to a reaction system for recycling through a pipeline 7, and the heavy components are discharged from the tower kettle through a pipeline 8 and flow into a heavy component residue tank V-3. Gaseous materials which are led out from the side line of the stripping section of the rectification main tower and carry metal ions and heavy components enter the bottom of a rectification side line tower TS-2 through a gas phase connecting pipeline 9 to be pressurized. In a side column, propylene glycol methyl ether acetate is further purified, heavy components which are subjected to mass transfer separation and carry metal ions are returned to a rectification separation main column through a side column bottom liquid connecting pipeline 10 and are discharged from a column bottom, propylene glycol methyl ether acetate is collected from the top of the side column and is also divided into two parts after being condensed by a condenser E-5, one part is returned to the top of the side column through a backflow pipeline 11, the other part is used as a product and enters a subsequent ion exchange resin bed CC through a pipeline 12 to further remove the metal ions, and finally, an electronic grade propylene glycol methyl ether acetate product flows into a product tank V-4 through a product pipeline 13.
The method for preparing the electronic grade propylene glycol monomethyl ether acetate by separation and purification comprises the following steps: the top of the dehydrating tower adopts normal pressure, the pressure value is about 0.1MPa, the temperature of the top of the dehydrating tower is 80-90 ℃, the preferred temperature is 88 ℃, and the reflux ratio of the dehydrating tower is 1.5-3; the pressure at the top of the main rectification and separation tower of the propylene glycol monomethyl ether acetate is 0.12-0.2MPa, the temperature at the top of the tower is 130-160 ℃, and the reflux ratio of the main rectification tower is 3-8; the pressure at the top of the propylene glycol methyl ether acetate side line tower is 0.1-0.18MPa, the temperature at the top of the tower is 130-170 ℃, and the reflux ratio of the side line tower is 0.5-2.
The present invention will be described in more detail with reference to examples
Example 1
The composition of the feed from the propylene glycol methyl ether acetate synthesis reactor is shown in the data in table 1,
TABLE 1 propylene glycol methyl ether acetate synthesis reactor outlet material composition
The separation and purification of propylene glycol methyl ether acetate is carried out by utilizing the process flow diagram shown in the attached figure 1, in the embodiment, a dehydrating tower, a propylene glycol methyl ether acetate rectification main tower and a side line tower all adopt packed towers, wherein the tower top pressure of the dehydrating tower is 0.1MPa, the reflux ratio of the dehydrating tower is 1.5, the tower top temperature of the dehydrating tower is 88 ℃, the tower top pressure of the propylene glycol methyl ether acetate rectification separation main tower is 0.12MPa, the corresponding tower top temperature is 134 ℃, the reflux ratio of the main tower is 6, the tower top pressure of the propylene glycol methyl ether acetate side line tower is 0.18MPa, the tower top temperature of the side line tower is 149 ℃, and the reflux ratio of the side line tower is 1.0. The acidity (calculated by acetic acid) of the propylene glycol monomethyl ether acetate product is less than 80ppm, the water content is less than 200ppm, and the content of each metal ion is less than 1 ppb.
Example 2
The feed composition is the same as that of example 1, and the separation and purification of propylene glycol methyl ether acetate is performed by using the process flow diagram shown in the attached figure 1, in this example, a dehydrating tower, a propylene glycol methyl ether acetate rectification main tower and a side line tower all adopt packed towers, wherein the tower top pressure of the dehydrating tower is 0.1MPa, the reflux ratio of the dehydrating tower is 3, the tower top temperature of the dehydrating tower is 90 ℃, the tower top pressure of the propylene glycol methyl ether acetate rectification separation main tower is 0.2MPa, the corresponding tower top temperature is 152 ℃, the reflux ratio of the main tower is 8, the tower top pressure of the propylene glycol methyl ether acetate side line tower is 0.18MPa, the tower top temperature of the side line tower is 167 ℃, and the reflux ratio of the side line tower is 2. The acidity (calculated by acetic acid) of the propylene glycol monomethyl ether acetate product is less than 300ppm, the water content is less than 180ppm, and the content of each metal ion is less than 1 ppb.
Example 3
The feed composition is the same as that of example 1, and the separation and purification of propylene glycol methyl ether acetate is performed by using the process flow diagram shown in the attached figure 1, in this example, a dehydrating tower, a propylene glycol methyl ether acetate rectification main tower and a side line tower all adopt packed towers, wherein the tower top pressure of the dehydrating tower is 0.1MPa, the reflux ratio of the dehydrating tower is 2, the tower top temperature of the dehydrating tower is 80 ℃, the tower top pressure of the propylene glycol methyl ether acetate rectification separation main tower is 0.12MPa, the corresponding tower top temperature is 146 ℃, the reflux ratio of the main tower is 3, the tower top pressure of the propylene glycol methyl ether acetate side line tower is 0.10MPa, the tower top temperature of the side line tower is 134 ℃, and the reflux ratio of the side line tower is 0.5. The acidity (calculated by acetic acid) of the propylene glycol methyl ether acetate product is less than 150ppm, the water content is less than 270ppm, and the content of each metal ion is less than 1 ppb.
In summary, the separation and purification method of electronic grade propylene glycol monomethyl ether acetate proposed by the present invention has been specifically described by the above preferred embodiments, but it should be understood that the above description should not be construed as limiting the present invention. All such similar substitutes and modifications apparent to those skilled in the art to which the invention pertains are deemed to be essential. Accordingly, the scope of the invention should be determined from the following claims.
Claims (4)
1. A purification method for preparing electronic grade propylene glycol methyl ether acetate is characterized in that a propylene glycol methyl ether acetate mixed material containing water, propylene glycol methyl ether and acetic acid at the outlet of a reactor is fed from the middle part of a dehydration tower, water is separated in the tower under the action of an entrainer and is extracted from the tower top, the dehydrated material is extracted from a tower bottom and is pumped into the middle part of a propylene glycol methyl ether acetate rectification main tower through a circulating pump, light and heavy components are separated, the unreacted raw material propylene glycol methyl ether, acetic acid and trace water mixture is distilled from the tower top and returned to the reactor for recycling, a gaseous mixture carrying metal ions and heavy components enters the bottom of a rectification side-line tower through a connecting pipeline, the propylene glycol methyl ether acetate migrates upwards in the tower, the heavy components and the metal ions return to the main tower and are discharged from the tower bottom through mass transfer separation, a propylene glycol methyl ether acetate product is extracted from the top of the side-line tower, and then enters an, obtaining an electronic grade propylene glycol methyl ether acetate product; the propylene glycol methyl ether acetate mixed material synthesized by the self-reactor enters from the middle part of a dehydration tower and is operated under normal pressure, the top pressure of the dehydration tower is 0.1MPa, the temperature at the top of the dehydration tower is 80-90 ℃, and the reflux ratio in the dehydration tower is 1.5-3; the dehydrated mixed material enters from the middle part of a propylene glycol methyl ether acetate rectification main tower, and the pressurization operation is adopted, wherein the pressure at the top of the propylene glycol methyl ether acetate rectification main tower is 0.12-0.2MPa, the temperature at the top of the propylene glycol methyl ether acetate rectification main tower is 130-160 ℃, and the reflux ratio of the main tower is 3-8; the propylene glycol methyl ether acetate and the entrained heavy components enter a side line tower through a connecting pipeline of a main tower and the side line tower, and the pressurization operation is adopted, wherein the tower top pressure of the propylene glycol methyl ether acetate side line tower is 0.10-0.18MPa, the tower top temperature is 130-170 ℃, and the reflux ratio of the side line tower is 0.5-2; the propylene glycol methyl ether acetate rectification side line tower is a purification tower only provided with a rectification section;
the entrainer is toluene, in the dehydration tower, the toluene and water form a lowest temperature azeotrope, the toluene and water are extracted from the top of the tower and enter a phase separation tank for phase separation, the upper layer of toluene phase returns to the dehydration tower, and the lower layer of water phase is extracted from the bottom; the side line tower and the product storage tank of the propylene glycol methyl ether acetate rectification main tower are made of stainless steel lining perfluoroalkoxy resin.
2. The method as set forth in claim 1, wherein the dehydration column, the propylene glycol methyl ether acetate rectification main column and the side column are plate columns or packed columns.
3. The method as set forth in claim 2, wherein when the dehydration column, the main rectification column and the side line column are all packed columns, the packing is plastic structured packing, ceramic structured packing or carbon fiber structured packing.
4. The method as set forth in claim 1, wherein said ion exchange resin bed is a strong acid type cation exchange resin.
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| CN109704959A (en) * | 2018-12-21 | 2019-05-03 | 江门谦信化工发展有限公司 | A kind of industrialized preparing process of electronic grade acetic acid ester solvent |
| CN112010754B (en) * | 2020-08-19 | 2023-02-28 | 江门谦信化工发展有限公司 | Refining method for esterification synthesis of ethylene glycol methyl ether acetate |
| CN112552174B (en) * | 2020-12-23 | 2023-04-11 | 江门谦信化工发展有限公司 | Device and method for rectifying acetic ester |
| CN114262269B (en) * | 2021-12-30 | 2023-09-26 | 宁波南大光电材料有限公司 | Preparation method of propylene glycol methyl ether acetate |
| CN116332736A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Recycling method of waste solvent in electronic industry |
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| CN101693661B (en) * | 2009-10-15 | 2012-09-05 | 无锡百川化工股份有限公司 | Method for producing propylene glycol methyl ether acetate |
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