CN114409500A - 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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- CN114409500A CN114409500A CN202210086550.4A CN202210086550A CN114409500A CN 114409500 A CN114409500 A CN 114409500A CN 202210086550 A CN202210086550 A CN 202210086550A CN 114409500 A CN114409500 A CN 114409500A
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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 176
- 239000007788 liquid Substances 0.000 title claims abstract description 75
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000010793 electronic waste Substances 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 41
- 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 11
- 238000000605 extraction Methods 0.000 claims description 7
- 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 2
- 239000000047 product Substances 0.000 description 22
- 238000009835 boiling Methods 0.000 description 19
- 229920002120 photoresistant polymer Polymers 0.000 description 11
- 239000000126 substance Substances 0.000 description 8
- 239000010408 film Substances 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 3
- 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
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011259 mixed solution Substances 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
- 230000006978 adaptation Effects 0.000 description 1
- 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
- 238000004821 distillation Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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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
- 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 no entrainer is introduced, the recovery of propylene glycol methyl ether and propylene glycol monomethyl ether acetate in the electronic waste liquid can be completed only by once vacuum rectification, the recovery rate of propylene glycol methyl ether and 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 methyl ether acetate from electronic waste liquid.
Background
In the electronics manufacturing industry and the optoelectronic industry, a mixture of propylene glycol methyl ether (PM) and propylene glycol monomethyl ether acetate (PMA) is often used in large amounts as a photoresist thinner, a photoresist remover, a photoresist stripping buffer, and a cleaning agent as a main component to remove esters such as photoresist on a panel. The reagent contains a large amount of PM and PMA in the used electronic waste liquid, and impurities such as water, photoresist and the like, so that the reagent has great harm to the environment, and the recycling of the PM and the PMA has high commercial value. At present, an entrainer which is added with water in the electronic waste liquid is commonly adopted in the industry to separate the water in the waste liquid so as to achieve the purpose of recovering PM and PMA. However, the entrainer is generally an organic solvent such as cyclohexane, normal hexane, isopropanol and the like, which not only causes great harm to the environment, but also causes complex process flow and large energy consumption of the method.
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 electronic waste liquid. According to the method, under the condition that no entrainer is introduced, PM and PMA in the electronic waste liquid can be continuously extracted only through once vacuum rectification, the recovery rate of the PM and the PMA is high, the purity of the obtained PM and PMA products is high, and the method is simple in process, high in production efficiency, low in energy consumption and environment-friendly.
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 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 vacuum rectification; collecting light components from the top of the rectifying tower, condensing part of the light components, refluxing the condensed light components to the rectifying tower, and circularly performing 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 feed inlet in the middle of the rectifying tower;
and collecting a target gas product at a side line extraction outlet of the rectifying tower, and condensing the target gas product to obtain anhydrous propylene glycol methyl ether and anhydrous propylene glycol monomethyl ether acetate.
According to the method, under the condition that no additional entrainer is introduced, the recovery of PM and PMA in the electronic waste liquid can be completed only through reduced pressure rectification, the purity of the obtained PM and PMA products is high, and the method is simple in process, high in production efficiency, low in energy consumption and environment-friendly.
Drawings
FIG. 1 is a process flow diagram for recovering PM and PMA according to example 1 of the present application;
FIG. 2 is a diagram of an apparatus according to an embodiment of the present application;
FIG. 3 is a process flow diagram for the recovery of PM and PMA of comparative example 1.
The reference numerals are explained below: 1-a rectifying tower; 2-a condenser; 3-a vacuum pump; 4-a reflux tank; 5-a product condenser; 6-product container; 7-a reboiler; 8-tower kettle circulating pump; a-a feed inlet; b-a side draw-off port; c-a tower top outlet; d, a tower top inlet; e-a tower bottom outlet.
Detailed Description
The technical scheme of the application is described in detail in the following with reference to the accompanying drawings.
First, the apparatus used in the embodiment of the present application will be described with reference to fig. 2. The rectifying tower 1 is an accommodating space formed by the top, the side wall and the bottom of the tower, and a feed inlet A and a lateral line extraction outlet B are arranged on the side wall of the rectifying tower 1. The feed inlet A is located in the middle of the rectifying tower 1, and the side draw outlet B is located in the middle-lower part of the rectifying tower 1 (i.e., the distance between the feed inlet and the top of the tower is smaller than the distance between the side draw outlet and the top of the tower). Wherein, the feed inlet A and the side draw-out port B can be on the same side of the rectifying tower 1 or not on the same side of the rectifying tower 1. The side draw-out port A is connected with the product condenser 5 through an 'n' type pipeline, the 'n' type pipeline is beneficial to the transportation of target gas products, and target liquid products obtained after condensation treatment can be conveyed to a product container 6 for storage. The top of the tower is provided with a tower top outlet C and a tower top inlet D, and the discharge port C is connected with a condenser 2, a vacuum pump 3 and a reflux tank 4 which are connected with each other. 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 a tower bottom discharge hole E is connected with a reboiler 7 and a tower kettle circulating pump 8 connected with the reboiler.
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 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 vacuum rectification; collecting light components from the top of the rectifying tower 1, condensing part of the light components, refluxing the condensed light components to the rectifying tower 1, and circularly performing 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) collecting a target gas product at a side line extraction outlet 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 is changed by controlling the pressure (negative pressure, namely less than 1 standard atmospheric pressure) in the rectifying tower 1, particularly the saturated vapor pressure of an azeotrope of water and PM is changed, so that the difference between the boiling point of the azeotrope and the boiling point of pure PM is enlarged, the amount of PM entrained when the azeotrope is evaporated out is reduced, and the loss of PM is reduced. Under the condition of reduced pressure, the temperature in the rectifying tower 1 increases from the tower top to the tower bottom, and the boiling points of the azeotrope of PM and water, PM and PMA also increase sequentially, so that the three substances can be vaporized at different positions in the rectifying tower 1, and the separation of water, PMA and partial PM is realized. While PMA and pure PM have relatively high boiling points, 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-out port B. And (3) conveying the target gas product to a condensing device for treatment through a pipeline after the target gas product is extracted, thus obtaining a mixed solution of the anhydrous PM and the anhydrous PMA. In addition, most of the light components will flow back to the rectification column 1, and the reflux can maintain the vacuum rectification continuously.
In conclusion, the method provided by the application can be used for completing the efficient and continuous recovery of PM and PMA by only using one reduced pressure rectifying tower under the condition of not introducing an entrainer, and is simple in process, high in production efficiency, low in energy consumption and environment-friendly.
In the actual production process, the electronic waste liquid enters the rectifying tower 1 from the feed inlet a, an azeotrope of water and PM in the electronic waste liquid is rectified at the middle upper part (part above the feed inlet) of the rectifying tower 1, and is taken out as a light component together with a small amount of low-boiling impurities from the tower top outlet C, and finally most of the light component flows back to the rectifying tower 1 through the condenser 2 and the reflux tank 4. And the anhydrous PM and the anhydrous PMA are rectified at the middle lower part (below a feed inlet and above the tower bottom) of the rectifying tower 1, and finally, a target gas product is extracted at a side draw-out port B, treated by a product condenser 5 and then transmitted to a product container 6 for storage. In addition, photoresist and other high boiling point impurities possibly existing in the electronic waste liquid can be extracted as heavy components at the bottom of the tower and conveyed to a recovery point for harmless treatment. Wherein, the low boiling point impurity and the high boiling point impurity comprise organic matters contained in reagents such as photoresistance thinner, photoresistance remover, photoresistance removing buffer solution, cleaning agent 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 liquid is not greater than 5%. The water content in the electronic waste liquid is controlled within the range, and the recovery rate of PM can be effectively ensured by the method.
In the embodiment of the application, the distance between the feed inlet A and the top of the tower is smaller than the distance between the side draw-out opening B and the top of the tower. The side line extraction 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, the rectification is carried out using a tray column. Illustratively, the plate column has a plate number of 50, the feed inlet A is the 20 th plate, and the side draw outlet B is provided at the 35 th plate. In other embodiments, the rectification is carried out using a packed column. Illustratively, the theoretical number of plates of the packed column is 50, the feed inlet A is the 20 th plate of the theoretical calculation, and the side draw outlet B is arranged at the 35 th plate of the theoretical calculation.
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). Illustratively, the absolute pressure in the rectifying column 1 may be 3kPa, 4kPa, 5kPa, 6kPa, 7kPa, 8kPa, 9kPa, 10kPa, 11kPa, 12kPa, 13kPa, 14kPa, 15 kPa. The pressure in the rectifying tower 1 is controlled within the range, the boiling points of all components in the electronic waste liquid can be effectively changed, so that the separation of water in the electronic waste liquid is realized, and the recovery of high-purity PM and PMA is completed. Generally, the smaller the pressure in the rectification column 1, the higher the degree of separation of the azeotrope from PM, and the lower the content of PM in the light component, the lower the rate of loss of PM.
In some embodiments of the present application, the ratio of the amount of liquid in the first portion to the amount of liquid in the second portion is (2-10): 1, i.e., a reflux ratio of (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 tower 1 under the corresponding reduced pressure condition can be maintained, the continuous rectification process can be ensured, and the balance among the product quality, the production efficiency and the production energy consumption can be achieved.
In the embodiment of the application, the temperature of the electronic waste liquid in the rectifying tower 1 is not more than 100 ℃. In the specific embodiment, in the rectification tower 1 under the reduced pressure, the boiling points of the azeotrope of PM and water, the PM and the PMA in the tower are all lower than 100 ℃. The temperature of the liquid in the rectifying tower 1 is controlled to be in the range, so that the temperature is higher than the boiling points of the three substances, and the higher recovery rate of PM and PMA is favorably ensured.
In some embodiments of the present application, the weight percentage of the propylene glycol methyl ether in the light component is 60% to 70%. The main component of the light fraction is an azeotrope of water and PM, the ratio of PM to water in the azeotrope being constant, but the azeotrope entrains additional PM during vaporization, resulting in loss of PM. The mass percent of PM in the light component is controlled within the range by controlling the condition of the vacuum distillation, so that the loss of PM can be reduced.
In the embodiment of the application, the purities of the anhydrous propylene glycol methyl ether and the anhydrous propylene glycol methyl ether acetate are more than or equal to 99.5%, and the industrial grade chemical standard can be achieved. 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%, and can reach the standard of electronic grade chemicals.
In the embodiment of the present application, the recovery rate of the propylene glycol methyl ether and the propylene glycol methyl ether acetate is more than 98%. The recovery rates of PM and PMA were (total mass of the obtained anhydrous PM and anhydrous PMA/total mass of PM and PMA in the electronic waste liquid) × 100%.
In some embodiments of the present application, before passing the electronic waste liquid into the rectifying tower 1, the electronic waste liquid is further subjected to a pretreatment, where the pretreatment includes treating the electronic waste liquid with a thin film evaporator to remove a part of impurities in the electronic waste liquid. The thin film evaporator may be a wiped film evaporator, and a scraper is provided in the wiped film evaporator. Introducing the electronic waste liquid into a wiped film evaporator, wherein low boiling point substances (including water, PM, PMA and low boiling point impurities) can be quickly evaporated, and sending the condensed low boiling point substances into a rectifying tower; high boiling point substances (photoresist and other high boiling point impurities) in the electronic waste liquid are remained in the wiped film evaporator. The photoresist has high viscosity and is easy to adhere to the wall of the wiped film evaporator, and the photoresist adhered to the wall of the wiped film evaporator can be wiped out by adopting the built-in scraper, so that the high heat transfer efficiency of the wiped film 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 in the subsequent vacuum rectification process, low boiling point impurities can be extracted from the top of the tower, trace high boiling point impurities are extracted from the bottom of the tower, and the energy consumption in the vacuum rectification process is further reduced.
The technical solution of the present application will be described in detail with reference to specific examples.
Example 1
And (3) feeding the electronic waste liquid into the rectifying tower 1 from the feeding hole, 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 ℃. Extracting light components from a second discharge hole at the top of the tower, condensing the light components by a condenser 3, conveying the first part into a reflux tank 4, conveying the first part to an inlet D at the top of the tower, and refluxing the first part into a rectifying tower 1; the second part is taken as waste liquid. The liquid amount ratio of the first portion to the second portion was 10: 1.
And a target gas product is extracted at a side line extraction port, treated by a product condenser 5 to obtain a mixed solution of anhydrous PM and anhydrous PMA, and transmitted 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 finally calculated to be 96.5%.
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 ℃. Finally, the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol monomethyl ether acetate is calculated to be 98.3%.
Example 3
The differences from example 1 are: controlling the absolute pressure in the rectifying tower to be 15 kPa. The temperature of the electronic waste liquid in the rectifying tower is 62.7 ℃.
The purity of the obtained anhydrous PM and the anhydrous PMA is 99.5%, and the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol methyl ether acetate is finally calculated to be 95.8%.
Example 4
The differences from example 1 are: the water content of the electronic waste liquid is 5 percent, and the absolute pressure in the rectifying tower is controlled to be 15 kPa. The temperature of the electronic waste liquid in the rectifying tower is 66.25 ℃.
The purity of the obtained anhydrous PM and the anhydrous PMA is 99.5%, and the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol methyl ether acetate is 98% by calculation.
Example 5
The differences from example 1 are: the liquid amount ratio of the first portion to the second portion in the condensed light component was 2: 1. The purity of the obtained anhydrous PM and the anhydrous PMA is 99.5%, and the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol methyl ether acetate is 95% through final calculation.
Example 6
The differences from example 1 are: the method also comprises the step of pretreating the electronic waste liquid, namely introducing the electronic waste liquid pretreated by the thin film evaporator into the rectifying tower 1 for reduced pressure distillation. The purity of the obtained anhydrous PM and the anhydrous PMA is 99.9%, and the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol methyl ether acetate is 96.4% by calculation.
In order to highlight the advantageous effects of the examples of the present application, the following comparative examples were provided.
Comparative example 1
Putting the electronic waste liquid into a mixing device, adding an impurity removal reactant cyclohexanone, and adding an entrainer cyclohexane after impurity removal. And introducing the waste liquid containing cyclohexane into a rectifying tower, and controlling the absolute pressure in the rectifying tower to be 150 kPa. Anhydrous propylene glycol methyl ether and anhydrous propylene glycol monomethyl ether acetate are extracted from a tower kettle of the rectifying tower.
Finally, the comprehensive recovery rate of the propylene glycol methyl ether and the propylene glycol methyl ether acetate is calculated to be 95%, and the purity is 99%.
According to the specific implementation conditions of the examples and the comparative examples, the continuous, high-efficiency and high-purity recovery of PM and PMA in the electronic waste liquid can be completed by only once vacuum rectification without introducing an entrainer. The method adopted in the comparative example 1 needs to add additional organic impurity removal agent and organic entrainer, is complex to operate, has high energy consumption and larger harm to the environment, and has the same production effect as the method adopted in the embodiment of the application. In conclusion, the technical scheme provided by the application has the advantages of simple process, high production efficiency, low energy consumption and environmental friendliness.
The foregoing is illustrative of the present application and it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the application and are intended to be within the scope of the application.
Claims (10)
1. A method for recovering propylene glycol methyl ether and propylene glycol methyl ether acetate from electronic waste liquid is characterized by comprising the following steps:
(1) providing 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 vacuum rectification; collecting light components from the top of the rectifying tower, condensing part of the light components, refluxing the condensed light components to the rectifying tower, and circularly performing 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 feed inlet in the middle of the rectifying tower;
and collecting a target gas product at a side line extraction outlet of the rectifying tower, and condensing the target gas product to obtain anhydrous propylene glycol methyl ether and anhydrous propylene glycol monomethyl ether acetate.
2. The method of claim 1, wherein the mass percent of water in the electronic waste liquid is not higher than 10%.
3. The method according to claim 1, characterized in that during the reduced pressure rectification the absolute pressure in the rectification column is 3-15 kPa.
4. The method of claim 1, wherein the temperature of the electronic waste liquid in the rectification column does not exceed 100 ℃.
5. The method of claim 1, wherein a first portion of the condensed light components is refluxed into the rectification column from the top of the rectification column, and a remaining second portion is withdrawn as a waste liquid.
6. The method according to claim 5, wherein the ratio of the amount of liquid of the first part to the amount of liquid of the second part is (2-10): 1.
7. the process of claim 1 wherein the distance between the feed inlet and the top of the column is less than the distance between the side draw outlet and the top of the column.
8. The method as claimed in claim 1, wherein the anhydrous propylene glycol methyl ether and the anhydrous propylene glycol methyl ether acetate have a purity of 99.5% or more.
9. The method of claim 1, wherein the recovery of the anhydrous propylene glycol methyl ether and the anhydrous propylene glycol methyl ether acetate is greater than 95%.
10. The method according to any one of claims 1 to 9, further comprising pretreating the electronic waste liquid before passing the electronic waste liquid into the rectifying tower, wherein the pretreating comprises treating the electronic waste liquid by using a thin film evaporator to remove part of impurities in the electronic waste liquid.
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| CN114989047A (en) * | 2022-07-21 | 2022-09-02 | 无锡中天固废处置有限公司 | Method for recovering dimethyl sulfoxide from waste organic solvent |
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