CN114409500B - Method for recovering propylene glycol methyl ether and propylene glycol monomethyl ether acetate from electronic waste liquid - Google Patents
Method for recovering propylene glycol methyl ether and propylene glycol monomethyl ether acetate from electronic waste liquid Download PDFInfo
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- CN114409500B CN114409500B CN202210086550.4A CN202210086550A CN114409500B CN 114409500 B CN114409500 B CN 114409500B CN 202210086550 A CN202210086550 A CN 202210086550A CN 114409500 B CN114409500 B CN 114409500B
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- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 title claims abstract description 178
- 239000007788 liquid Substances 0.000 title claims abstract description 74
- 239000010793 electronic waste Substances 0.000 title claims abstract description 66
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000011084 recovery Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000012535 impurity Substances 0.000 claims description 20
- 238000010992 reflux Methods 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 6
- QMYDVDBERNLWKB-UHFFFAOYSA-N propane-1,2-diol;hydrate Chemical compound O.CC(O)CO QMYDVDBERNLWKB-UHFFFAOYSA-N 0.000 claims description 5
- 239000010409 thin film Substances 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 23
- 238000009835 boiling Methods 0.000 description 18
- 229920002120 photoresistant polymer Polymers 0.000 description 14
- 239000000126 substance Substances 0.000 description 8
- 230000001276 controlling effect Effects 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 4
- 238000007790 scraping Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- DQYBDCGIPTYXML-UHFFFAOYSA-N ethoxyethane;hydrate Chemical compound O.CCOCC DQYBDCGIPTYXML-UHFFFAOYSA-N 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Classifications
-
- 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
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application provides a method for recovering propylene glycol methyl ether and propylene glycol monomethyl ether acetate from electronic waste liquid. According to the method, under the condition that an entrainer is not introduced, the recovery of propylene glycol methyl ether and propylene glycol monomethyl ether acetate in the electronic waste liquid can be completed only by one-time reduced pressure rectification, the recovery rate of the propylene glycol methyl ether and the propylene glycol monomethyl ether acetate is high, and the purity of the obtained propylene glycol methyl ether and propylene glycol monomethyl ether acetate products is high. The method has the advantages of simple process, high production efficiency, low energy consumption and environmental friendliness.
Description
Technical Field
The application relates to the technical field of chemical recovery, in particular to a method for recovering propylene glycol methyl ether and propylene glycol monomethyl ether acetate from electronic waste liquid.
Background
In the fields of electronic manufacturing industry and photoelectric industry, a mixed solution of propylene glycol methyl ether (PM) and propylene glycol monomethyl ether acetate (PMA) is often used as a photoresist diluent, a photoresist remover, a photoresist removing buffer solution and a cleaning agent in large quantities to remove ester substances such as photoresist on a panel. The reagent contains a large amount of PM and PMA, water, photoresist and other impurities in the electronic waste liquid after use, so that the reagent has great harm to the environment, and the recycling of PM and PMA has high commercial value. At present, the water in the waste liquid is separated by adding an entrainer of water into the electronic waste liquid, so as to achieve the aim of recovering PM and PMA. However, the entrainer is generally an organic solvent such as cyclohexane, n-hexane, isopropanol and the like, which has great harm to the environment, and the method has complicated process flow and high energy consumption.
Disclosure of Invention
In view of this, the present application provides a method for recovering propylene glycol methyl ether and propylene glycol monomethyl ether acetate from an electronic waste liquid. Under the condition of no entrainer, PM and PMA in the electronic waste liquid can be continuously extracted by only one-time vacuum rectification, the recovery rate of PM and PMA is high, the purity of the obtained PM and PMA products is high, and the method has the advantages of simple process, high production efficiency, low energy consumption and environmental friendliness.
Specifically, the application provides a method for recovering propylene glycol methyl ether and propylene glycol monomethyl ether acetate from electronic waste liquid, which comprises the following steps:
(1) Providing an electronic waste liquid, wherein the electronic waste liquid contains propylene glycol methyl ether, propylene glycol monomethyl ether acetate, water and impurities;
(2) Introducing the electronic waste liquid into a rectifying tower for reduced pressure rectification; extracting light components from the top of the rectifying tower, condensing part of the light components, refluxing the condensed light components into the rectifying tower, and circularly carrying out the reduced pressure rectification; wherein the light component comprises the propylene glycol methyl ether and water; the electronic waste liquid is introduced into the rectifying tower from a feeding port in the middle of the rectifying tower;
and extracting a target gas product from a side extraction port of the rectifying tower, and condensing the target gas product to obtain anhydrous propylene glycol methyl ether and anhydrous propylene glycol monomethyl ether acetate.
The method can recover PM and PMA in the electronic waste liquid only by vacuum rectification without introducing extra entrainer, and the obtained PM and PMA products have high purity, and the method has simple process, high production efficiency, low energy consumption and environmental friendliness.
Drawings
FIG. 1 is a process flow diagram for PM and PMA recovery in example 1 of the present application;
FIG. 2 is a device diagram of an embodiment of the present application;
fig. 3 is a process flow diagram for PM and PMA recovery in comparative example 1.
The reference numerals are explained as follows: 1-a rectifying tower; a 2-condenser; 3-a vacuum pump; 4-a reflux drum; 5-a product condenser; 6-a product container; 7-reboiler; 8-a tower kettle circulating pump; a-a feed inlet; b-side draw; c-an overhead outlet; d-tower top inlet; e-bottom outlet.
Detailed Description
The following describes the technical scheme of the application in detail with reference to the accompanying drawings.
First, the apparatus used in the embodiment of the present application is described with reference to fig. 2. The rectifying tower 1 is an accommodating space formed by a tower top, a side wall and a tower bottom, and a feed inlet A and a side draw outlet B are arranged on the side wall of the rectifying tower 1. The above-mentioned feed port a is located in the middle of the rectifying column 1, and the side draw port B is located in the middle lower part of the rectifying column 1 (i.e., the distance between the feed port and the column top is smaller than the distance between the side draw port and the column top). The feed port a and the side draw port B may be on the same side of the rectifying column 1 or may not be on the same side of the rectifying column 1. The side draw outlet A is connected with the product condenser 5 through an n-shaped pipeline, the n-shaped pipeline is favorable for conveying target gas products, and the target liquid products obtained after condensation treatment can be conveyed into the product container 6 for storage. The tower top is provided with a tower top outlet C and a tower top inlet D, and the discharge port C is connected with the condenser 2 and the vacuum pump 3 and the reflux tank 4 which are connected. The absolute pressure in the rectification column 1 can be regulated by means of a vacuum pump 3. The tower bottom is provided with a tower bottom outlet E, and the tower bottom outlet E is connected with a reboiler 7 and a connected tower kettle circulating pump 8.
Specifically, the embodiment of the application provides a method for recovering propylene glycol methyl ether and propylene glycol monomethyl ether acetate from electronic waste liquid, which comprises the following steps:
(1) Providing an electronic waste liquid, wherein the electronic waste liquid contains propylene glycol methyl ether, propylene glycol monomethyl ether acetate, water and impurities;
(2) Introducing the electronic waste liquid into a rectifying tower 1 for reduced pressure rectification; extracting light components from the top of the rectifying tower 1, condensing part of the light components, refluxing the condensed light components into the rectifying tower 1, and circularly carrying out the reduced pressure rectification; wherein the light component comprises the propylene glycol methyl ether and water; the electronic waste liquid is introduced into the rectifying tower 1 from a feed inlet A in the middle of the rectifying tower 1;
and (3) extracting a target gas product from a side extraction port of the rectifying tower 1, and condensing the target gas product to obtain anhydrous propylene glycol methyl ether and anhydrous propylene glycol monomethyl ether acetate.
The electronic waste liquid contains water, PM, PMA and a small amount of impurities (including photoresist and other organic solvents), and the PM can be dissolved in the water and can form an azeotrope with the water. In the application, the saturated vapor pressure of each component in the electronic waste liquid, especially the saturated vapor pressure of the azeotrope of water and PM is changed by controlling the pressure (negative pressure, namely, less than 1 standard atmosphere) in the rectifying tower 1, so that the difference between the boiling point of the azeotrope and the boiling point of pure PM is increased, the amount of PM entrained when the azeotrope is distilled out is reduced, and the loss of PM is reduced. The temperature in the rectifying tower 1 increases from the top to the bottom under the condition of reduced pressure, and the boiling points of the azeotrope of PM and water, PM and PMA also increase in sequence, so that the three substances can be gasified at different positions in the rectifying tower 1, and the separation of water, PMA and part of PM is realized. While the boiling points of PMA and pure PM are relatively high, they are vaporized in the middle lower part of the rectifying column 1 (i.e., the part between the feed port and the bottom of the column), and the target gas product (mixed vapor of PM and PMA) is accumulated at the side draw port B. And (3) after the target gas product is extracted, transporting the extracted target gas product to a condensing device for treatment through a pipeline, and obtaining the mixed solution of the anhydrous PM and the anhydrous PMA. In addition, most of the light components can flow back to the rectifying tower 1, and the reflux can maintain the continuous operation of the reduced pressure rectification.
In summary, the method provided by the application can complete the efficient and continuous recovery of PM and PMA by using only one decompression rectifying tower under the condition of not introducing an entrainer, and has the advantages of simple process, high production efficiency, low energy consumption and environmental friendliness.
In the actual production process, the electronic waste liquid enters the rectifying tower 1 from the feed inlet A, the azeotrope of water and PM in the electronic waste liquid is rectified at the middle upper part (the part above the feed inlet) of the rectifying tower 1, and is taken out of the tower top outlet C as a light component together with a small amount of low-boiling impurities, and then flows back to the rectifying tower 1 through the condenser 2 and the reflux tank 4, and finally most of the light component flows back to the rectifying tower 1. The anhydrous PM and the anhydrous PMA are rectified at the middle lower part (below the feed inlet and above the bottom of the tower) of the rectifying tower 1, and finally target gas products are extracted at a side-draw outlet B and are transmitted to a product container 6 for storage after being processed by a product condenser 5. In addition, photoresist and other high boiling impurities which may be present in the electronic waste liquid are extracted as a heavy component at the bottom of the tower and transported to a recovery point for innocent treatment. Wherein the low boiling point impurities and the high boiling point impurities comprise organic matters contained in reagents such as photoresist diluents, photoresist removers, photoresist removing buffers, cleaning agents and the like.
In some embodiments of the present application, the mass percentage of the water in the electronic waste liquid is not higher than 10%. In some embodiments, the mass percent of the water in the electronic waste is not higher than 5%. The water content in the electronic waste liquid is controlled in the range, and the recovery rate of PM can be effectively ensured by using the method.
In the embodiment of the application, the distance between the feeding port A and the tower top is smaller than the distance between the side drawing port B and the tower top. And the side draw-out port B is arranged at a proper position, so that the high-quality and high-efficiency extraction of PM and PMA products can be ensured. In some embodiments of the present application, rectification is performed using tray columns. Illustratively, the tray number of the tray column is 50, the feed inlet A is the 20 th tray, and the side offtake B is disposed at the 35 th tray. In other embodiments, the rectification is performed using a packed column. Illustratively, the packing tower has a theoretical calculation plate number of 50, the feed inlet A is the theoretical calculation 20 th plate, and the side offtake B is arranged at the theoretical calculation 35 th plate.
In the present embodiment, the absolute pressure in the rectifying column 1 is 3kPa to 15kPa (i.e., the gauge pressure of the vacuum gauge is-98 kPa to-86 kPa). For example, the absolute pressure in the rectifying column 1 may be 3kPa, 4kPa, 5kPa, 6kPa, 7kPa, 8kPa, 9kPa, 10kPa, 11kPa, 12kPa, 13kPa, 14kPa, 15kPa. The pressure in the rectifying tower 1 is controlled within the range, so that the boiling points of all components in the electronic waste liquid can be effectively changed, the separation of water in the electronic waste liquid is realized, and the recovery of PM and PMA with high purity is completed. In general, the smaller the pressure in the rectifying column 1, the higher the degree of separation of the azeotrope from the PM, the lower the content of PM in the light component, and the lower the loss rate of PM.
In some embodiments of the present application, the ratio of the liquid amount of the first portion to the liquid amount of the second portion is (2-10): 1, i.e. the reflux ratio is (2-10): 1. the liquid amounts (reflux ratio) of the two parts are controlled within the above range, so that the rectification environment in the rectification column 1 under the corresponding reduced pressure condition can be maintained, the continuous rectification process can be ensured, and the balance between the product quality, the production efficiency and the production energy consumption can be achieved.
In this embodiment, the temperature of the electronic waste liquid in the rectifying tower 1 does not exceed 100 ℃. In a specific embodiment, in the rectifying tower 1 under the condition of reduced pressure, the boiling points of azeotropes of PM and water, PM and PMA in the tower are all lower than 100 ℃. The liquid temperature in the rectifying tower 1 is controlled within the range, so that the liquid temperature is higher than the boiling points of the three substances, and the higher recovery rate of PM and PMA is ensured.
In some embodiments of the present application, the mass percentage of the propylene glycol methyl ether in the light component is 60% -70%. The main component of the light component is an azeotrope of water and PM, the proportion of PM to water in the azeotrope is constant, but the azeotrope can entrain extra PM in the vaporization process, so that PM is lost. By controlling the conditions of the reduced pressure rectification and controlling the mass percentage of PM in the light component within the above-described range, the loss of PM can be reduced.
In the embodiment of the application, the purity of the anhydrous propylene glycol methyl ether and the purity of the anhydrous propylene glycol monomethyl ether acetate are greater than or equal to 99.5%, and can reach the industrial grade chemical standard. In some embodiments, the purity of the anhydrous propylene glycol methyl ether and the anhydrous propylene glycol monomethyl ether acetate is greater than or equal to 99.9%, which can meet electronic grade chemical standards.
In embodiments of the present application, the recovery rate of propylene glycol methyl ether and propylene glycol monomethyl ether acetate is greater than 98%. Recovery rate of PM and pma= (sum of mass of anhydrous PM and anhydrous PMA obtained/sum of mass of PM and PMA in the aforementioned electronic waste liquid) ×100%.
In some embodiments of the present application, before the electronic waste is introduced into the rectifying tower 1, the method further comprises pretreating the electronic waste, where the pretreatment includes treating the electronic waste with a thin film evaporator to remove a portion of impurities in the electronic waste. The thin film evaporator can be a film scraping evaporator, and a scraper is arranged in the film scraping evaporator. Introducing the electronic waste liquid into a wiped film evaporator, quickly evaporating low boiling point substances (including water, PM, PMA and low boiling point impurities) in the electronic waste liquid, condensing the electronic waste liquid, and then sending the electronic waste liquid into a rectifying tower; and high boiling point substances (photoresist and other high boiling point impurities) in the electronic waste liquid remain in the wiped film evaporator. The photoresist has high viscosity and is easy to be adhered to the wall of the film scraping evaporator, and the photoresist adhered to the wall can be scraped by adopting a built-in scraper, so that the high heat transfer efficiency of the film scraping evaporator is ensured. The photoresist and most other high boiling point impurities in the electronic waste liquid can be removed in the pretreatment process, and the content of the impurities in the pretreated electronic waste liquid is extremely low, so that the low boiling point impurities can be extracted from the tower top in the subsequent vacuum rectification process, and trace high boiling point impurities can be extracted from the tower bottom, thereby further reducing the energy consumption in the vacuum rectification process.
The following describes the technical scheme of the present application in detail with reference to specific embodiments.
Example 1
And sending the electronic waste liquid into the rectifying tower 1 from a feed inlet, and controlling the absolute pressure in the rectifying tower to be 3kPa by regulating and controlling the parameters of the vacuum pump 2. Wherein the water content of the electronic waste liquid is 10%, and the temperature of the electronic waste liquid in the rectifying tower is 32.2 ℃. Light components are extracted from a second discharge hole at the top of the tower, condensed by a condenser 3, and the first part enters a reflux tank 4 and is conveyed to an inlet D at the top of the tower to be refluxed into a rectifying tower 1; the second fraction is withdrawn as waste liquid. The ratio of the liquid amount of the first part to the liquid amount of the second part is 10:1.
And (3) extracting a target gas product from a side extraction port, processing the target gas product by a product condenser 5 to obtain a mixed solution of anhydrous PM and anhydrous PMA, and transmitting the mixed solution to a product container 6 for storage.
The purity of the anhydrous PM and the anhydrous PMA is 99.5%, and the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol monomethyl ether acetate is 96.5% finally calculated.
Example 2
The differences from example 1 are: the water content of the electronic waste liquid is 5%, the purity of the obtained anhydrous PM and anhydrous PMA is 99.5%, and the temperature of the electronic waste liquid in the rectifying tower is 34.8 ℃. And finally, calculating to obtain the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol monomethyl ether acetate of 98.3%.
Example 3
The differences from example 1 are: the absolute pressure in the rectifying tower is controlled to be 15kPa. The temperature of the electronic waste liquid in the rectifying tower is 62.7 ℃.
The purity of the obtained anhydrous PM and the purity of the obtained anhydrous PMA are 99.5%, and the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol monomethyl ether acetate is 95.8% finally calculated.
Example 4
The differences from example 1 are: the water content of the electronic waste liquid is 5%, and the absolute pressure in the rectifying tower is controlled to be 15kPa. The temperature of the electronic waste liquid in the rectifying tower is 66.25 ℃.
The purity of the obtained anhydrous PM and the purity of the obtained anhydrous PMA are 99.5%, and the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol monomethyl ether acetate is 98% finally calculated.
Example 5
The differences from example 1 are: in the condensed light component, the liquid amount ratio of the first part to the second part is 2:1. The purity of the obtained anhydrous PM and the purity of the obtained anhydrous PMA are 99.5%, and the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol monomethyl ether acetate is 95% finally calculated.
Example 6
The differences from example 1 are: the method also comprises the step of preprocessing the electronic waste liquid, namely, introducing the electronic waste liquid obtained after the pretreatment of the thin film evaporator into the rectifying tower 1 for reduced pressure distillation. The purity of the obtained anhydrous PM and the purity of the obtained anhydrous PMA are 99.9%, and the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol monomethyl ether acetate is 96.4% finally calculated.
To highlight the beneficial effects of the embodiments of the present application, the following comparative examples are set forth.
Comparative example 1
Placing the electronic waste liquid in a mixing device, adding impurity removing reactant-cyclohexanone, and adding entrainer-cyclohexane after impurity removal. Introducing the waste liquid containing cyclohexane into a rectifying tower, and controlling the absolute pressure in the rectifying tower to be 150kPa. And (3) extracting anhydrous propylene glycol methyl ether and anhydrous propylene glycol monomethyl ether acetate from the tower bottom of the rectifying tower.
And finally, the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol monomethyl ether acetate is calculated to be 95%, and the purity is 99%.
As can be seen from the specific implementation cases of the examples and the comparative examples, the continuous, efficient and high-purity recovery of PM and PMA in the electronic waste liquid can be completed by only one-time vacuum rectification under the condition that the entrainer is not introduced. The method adopted in the comparative example 1 needs to add additional organic impurity removing agent and organic entrainer, has complicated operation, high energy consumption and larger harm to the environment, and the obtained production effect is equivalent to that of the embodiment of the application. In summary, it can be seen that the technical scheme provided by the application is simple in process, high in production efficiency, low in energy consumption and environment-friendly.
While the foregoing is directed to exemplary embodiments of the present application, it will be appreciated by those of ordinary skill in the art that numerous modifications and variations can be made thereto without departing from the principles of the present application, and such modifications and variations are to be regarded as being within the scope of the present application.
Claims (4)
1. A method for recovering propylene glycol methyl ether and propylene glycol monomethyl ether acetate from an electronic waste liquid, which is characterized by comprising the following steps:
(1) Providing an electronic waste liquid, wherein the electronic waste liquid contains propylene glycol methyl ether, propylene glycol monomethyl ether acetate, water and impurities;
(2) Introducing the electronic waste liquid into a rectifying tower for reduced pressure rectification, and controlling the absolute pressure in the rectifying tower to be 3kPa-15kPa, wherein the temperature of the electronic waste liquid in the rectifying tower is not more than 100 ℃; extracting light components from the top of the rectifying tower, condensing part of the light components, refluxing the condensed light components into the rectifying tower, and circularly carrying out the reduced pressure rectification; wherein the light component comprises the propylene glycol methyl ether and water;
wherein, a first part of the condensed light components flows back to the rectifying tower from the top of the rectifying tower, and the remaining second part is extracted as waste liquid; the ratio of the liquid amount of the first portion to the liquid amount of the second portion is (2-10): 1, a step of; wherein the mass percentage of propylene glycol methyl ether in the light component is 60% -70%;
the electronic waste liquid is introduced into the rectifying tower from a feeding port in the middle of the rectifying tower; the distance between the feeding port and the tower top is smaller than the distance between the side line extraction port and the tower top;
extracting a target gas product from a side extraction port of the rectifying tower, and condensing the target gas product to obtain anhydrous propylene glycol methyl ether and anhydrous propylene glycol monomethyl ether acetate;
before the electronic waste liquid is introduced into the rectifying tower, the method further comprises the step of pretreating the electronic waste liquid, wherein the pretreatment comprises the step of treating the electronic waste liquid by adopting a thin film evaporator so as to remove part of impurities in the electronic waste liquid.
2. The method of claim 1, wherein the mass percent of water in the electronic waste is no greater than 10%.
3. The method of claim 1, wherein the purity of the anhydrous propylene glycol methyl ether and the anhydrous propylene glycol monomethyl ether acetate is 99.5% or greater.
4. The method of claim 1, wherein the combined recovery of the anhydrous propylene glycol methyl ether and the anhydrous propylene glycol monomethyl ether acetate is 95.8%.
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| CN203494192U (en) * | 2013-08-22 | 2014-03-26 | 无锡中天固废处置有限公司 | Device for continuously recovering propylene glycol monomethyl ether and propylene glycol methyl ether acetate |
| CN109265314A (en) * | 2018-11-28 | 2019-01-25 | 临沂中天环保科技有限公司 | The preparation method and preparation facilities of propylene glycol methyl ether acetate |
| CN109796335A (en) * | 2019-01-08 | 2019-05-24 | 江门谦信化工发展有限公司 | A kind of method of high efficiency joint production of propylene glycol methyl ether and propylene glycol methyl ether acetate |
| CN110204442A (en) * | 2019-05-23 | 2019-09-06 | 安徽京控环境技术服务有限公司 | A method of purification propylene glycol methyl ether acetate is recycled from spent organic solvent |
| CN112194580A (en) * | 2020-11-04 | 2021-01-08 | 中建安装集团有限公司 | Device and process for producing propylene glycol monomethyl ether acetate by reactive distillation coupled pervaporation |
| CN113527072A (en) * | 2021-06-17 | 2021-10-22 | 四川熔增环保科技有限公司 | Method for recovering and purifying propylene glycol monomethyl ether and propylene glycol monomethyl ether acetate from electronic waste liquid |
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