CN112044419B - Method for regenerating resin in isopropanol recovery process - Google Patents
Method for regenerating resin in isopropanol recovery process Download PDFInfo
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- CN112044419B CN112044419B CN202010871521.XA CN202010871521A CN112044419B CN 112044419 B CN112044419 B CN 112044419B CN 202010871521 A CN202010871521 A CN 202010871521A CN 112044419 B CN112044419 B CN 112044419B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3458—Regenerating or reactivating using a particular desorbing compound or mixture in the gas phase
- B01J20/3466—Regenerating or reactivating using a particular desorbing compound or mixture in the gas phase with steam
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3425—Regenerating or reactivating of sorbents or filter aids comprising organic materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
Abstract
The invention provides a method for regenerating resin in an isopropanol recovery process, which comprises the following steps: using the pretreated first crude isopropanol to carry out solvent regeneration on the adsorbed resin; and then, steam is adopted to carry out steam regeneration on the resin after solvent regeneration, wherein the first crude isopropanol regenerates the resin, the purposes of effectively regenerating the resin and treating waste with waste are achieved, the steam regeneration is used to play roles of cleaning residual isopropanol and deeply regenerating, the resin has long cycle service life, and the cost of the isopropanol recovery process is reduced.
Description
Technical Field
The invention relates to the technical field of waste liquid treatment, in particular to a method for regenerating resin in an isopropanol recovery process.
Background
Isopropyl alcohol is an organic compound, an isomer of n-propyl alcohol, and is also referred to as IPA in industry, which is colorless transparent liquid, has smell similar to a mixture of ethanol and acetone, is soluble in water, and is also soluble in most organic solvents such as alcohol, ether, benzene and chloroform, and isopropyl alcohol is an important chemical product and raw material.
At present, in the electronic industry or the printing industry, isopropanol is often used as a cleaning liquid, and the isopropanol cleaning waste liquid contains more isopropanol and is difficult to recycle, so that the production cost is increased, and the environmental pollution is large or the waste water is difficult to post-treat.
CN2539738Y discloses a device for extracting isopropyl alcohol from waste liquid for cleaning printing plates, and CN1249294a discloses a method for refining isopropyl alcohol by a combined process of salt extraction and azeotropic distillation, which uses a rectification mode to recover high-purity isopropyl alcohol, but does not mention how to dispose of isopropyl alcohol mother liquor.
CN102173521B discloses a method for treating high-concentration industrial wastewater containing isopropyl alcohol, which uses a catalytic oxidation method to treat the isopropyl alcohol wastewater, but because isopropyl alcohol is easy to volatilize, an aeration mode can produce isopropyl alcohol waste gas, so that secondary pollution is caused.
CN104525114B discloses a method for treating isopropyl alcohol wastewater by using modified activated carbon, which utilizes modified activated carbon to adsorb isopropyl alcohol wastewater, but the initial COD value that can be treated is low, and the activated carbon needs to be regenerated at high temperature, which has high requirements on equipment.
Therefore, there is a need to develop a method for recovering isopropanol to achieve the purposes of reducing cost and reducing emissions.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a method for regenerating resin in the process of recovering isopropanol, which regenerates the resin through first coarse isopropanol, achieves the purposes of effectively regenerating the resin and treating waste with waste, and uses steam for regeneration to play roles of cleaning residual isopropanol and deeply regenerating, so that the recycling service life of the resin is long, and the cost of the process of recovering isopropanol is reduced.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for resin regeneration in an isopropanol recovery process, the method comprising: using the pretreated first crude isopropanol to carry out solvent regeneration on the adsorbed resin; and then steam is adopted to carry out steam regeneration on the resin after the solvent regeneration.
According to the invention, the resin is regenerated through the first crude isopropanol, the purposes of effectively regenerating the resin and treating waste by waste are achieved, and steam regeneration is used for cleaning residual isopropanol and deeply regenerating, so that compared with pure steam regeneration, the cycle service life of the resin is prolonged; compared with the regeneration of the pure solvent, the method reduces the regeneration cost, has no problem of the treatment of the regenerated solvent, and has higher economic benefit and environmental protection benefit.
Preferably, the mass percentage of the isopropanol in the first crude isopropanol is 55-65 wt%, for example, 55wt%, 56wt%, 57wt%, 58wt%, 59wt%, 60wt%, 61wt%, 62wt%, 63wt%, 64wt%, 65wt%, or the like.
Preferably, the resin comprises macroporous resin.
Preferably, the temperature of the solvent regeneration is 5 to 45 ℃, and for example, 5 ℃, 10 ℃, 12 ℃, 15 ℃, 18 ℃, 20 ℃, 22 ℃, 25 ℃, 28 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃ or the like can be used.
Preferably, the flow rate of the first crude isopropanol in the solvent regeneration is 0.5-2 BV/h, and can be, for example, 0.5BV/h, 0.8BV/h, 0.9BV/h, 1.0BV/h, 1.2BV/h, 1.3BV/h, 1.5BV/h, 1.8BV/h, 2BV/h, or the like.
Preferably, the amount of the first crude isopropyl alcohol used in the solvent regeneration is 0.5 to 3 times the volume of the resin, and may be, for example, 0.5 times, 0.8 times, 1.0 times, 1.2 times, 1.5 times, 1.8 times, 2 times, 2.5 times, 3 times, or the like.
Preferably, the steam regeneration temperature is 120 to 180 ℃, and may be 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 160 ℃, 165 ℃, 170 ℃, 175 ℃, 180 ℃, or the like, for example.
The method strictly controls the steam regeneration temperature to be 120-180 ℃, has low energy consumption, can deeply regenerate and has little damage to resin.
Preferably, the mass of the steam in the steam regeneration is 2 to 4kg, and may be, for example, 2kg, 2.2kg, 2.3kg, 2.4kg, 2.5kg, 2.7kg, 2.8kg, 3kg, 3.2kg, 3.5kg, 3.8kg, or 4kg.
Preferably, the pressure of the steam regeneration is 0.2 to 0.4kPa, for example, 0.2kPa, 0.22kPa, 0.25kPa, 0.26kPa, 0.28kPa, 0.3kPa, 0.32kPa, 0.35kPa, 0.38kPa, or 0.4kPa, etc. may be used.
As a preferred technical solution of the present invention, the method includes: using the pretreated first crude isopropanol to carry out solvent regeneration on the adsorbed resin; then steam is adopted to carry out steam regeneration on the resin after the solvent regeneration; the regeneration temperature of the solvent is 5-45 ℃, the flow of the first crude isopropanol is 0.5-2 BV/h, and the dosage of the first crude isopropanol is 0.5-3 times of the volume of the resin; the temperature of steam regeneration is 120-180 ℃, the mass of steam is 2-4 kg, and the pressure is 0.2-0.4 kPa.
In a second aspect, the present invention provides a method for recovering isopropanol from isopropanol waste liquid, wherein the method adopts the method for regenerating resin in the isopropanol recovery process in the first aspect to regenerate resin.
The method for recovering the isopropanol from the isopropanol waste liquid adopts the special resin regeneration process, prolongs the cycle service life of the resin, and greatly reduces the recovery cost of the isopropanol.
Preferably, the method comprises the steps of:
(1) Pretreating the isopropanol waste liquid to obtain isopropanol pretreatment mother liquor and first crude isopropanol;
(2) The isopropanol pretreatment mother liquor in the step (1) is adsorbed by resin to obtain adsorption effluent;
(3) Performing solvent regeneration on the resin adsorbed in the step (2) by using the first crude isopropanol in the step (1) to obtain second crude isopropanol;
the resin after the solvent regeneration is recycled to the step (2) for resin adsorption after the steam regeneration;
(4) And refining the first crude isopropanol and the second crude isopropanol to obtain an isopropanol product.
Preferably, the mass percentage of the isopropanol in the isopropanol waste liquid in the step (1) is 10-40 wt%, for example, 10wt%, 12wt%, 15wt%, 18wt%, 20wt%, 22wt%, 25wt%, 28wt%, 30wt%, 32wt%, 33wt%, 35wt%, 38wt%, 40wt%, or the like.
The isopropanol waste liquid is mainly water, the isopropanol content is 10-40 wt%, and the isopropanol waste liquid also contains a small amount of organic matters and the like.
The source of the isopropyl alcohol waste liquid is not particularly limited, and may be, for example, an electronic device cleaning waste liquid and/or a cleaning liquid in the production process thereof, and the like.
Preferably, the pretreatment in step (1) comprises rectification.
The rectification is not particularly limited in the present invention, and rectification which is well known to those skilled in the art and can primarily separate water and isopropyl alcohol may be employed.
Preferably, the mass percentage of the isopropanol in the first crude isopropanol is 55-65 wt%, for example, 55wt%, 56wt%, 57wt%, 58wt%, 59wt%, 60wt%, 61wt%, 62wt%, 63wt%, 64wt%, 65wt%, or the like.
Preferably, the resin in step (2) comprises a macroporous resin.
Preferably, the pore diameter of the macroporous resin is 100-1000 nm, for example, 100nm, 200nm, 300nm, 400nm, 500nm, 600nm, 700nm, 800nm, 900nm or 1000nm, etc.
Preferably, the mass percentage of the isopropyl alcohol in the isopropyl alcohol pretreatment mother liquor is 0.5-1%, for example, 0.5%, 0.6%, 0.7%, 0.75%, 0.8%, 0.85%, 0.9%, 0.95% or 1%.
Preferably, the chemical oxygen demand in the isopropanol pretreatment mother liquor is 4000-10000 mg/L, for example, 4000mg/L, 4500mg/L, 5000mg/L, 5500mg/L, 6000mg/L, 6500mg/L, 7000mg/L, 7500mg/L, 8000mg/L, 8500mg/L, 9000mg/L, 9500mg/L, 10000mg/L, etc.
Preferably, the chemical oxygen demand of the adsorbed effluent is less than 500mg/L, and can be 499mg/L, 495mg/L, 490mg/L, 470mg/L, 450mg/L, 440mg/L, 400mg/L, 380mg/L, 350mg/L, 300mg/L, etc.
Preferably, the temperature of the adsorption in the step (2) is 5 to 45℃and may be, for example, 5℃10℃15℃20℃25℃30℃35℃40℃45 ℃.
Preferably, the flow rate of the isopropyl alcohol pretreatment mother liquor in the adsorption is 0.5-2 BV/h, for example, 0.5BV/h, 0.7BV/h, 0.8BV/h, 0.9BV/h, 1.0BV/h, 1.2BV/h, 1.5BV/h, 1.8BV/h or 2BV/h, etc.
Preferably, the steam condensate after steam regeneration in the step (3) is mixed with the isopropanol waste liquid in the step (1).
Preferably, the mass percentage of the isopropanol in the steam condensate water is 1-2 wt%, for example, 1wt%, 1.1wt%, 1.2wt%, 1.3wt%, 1.4wt%, 1.5wt%, 1.6wt%, 1.7wt%, 1.8wt%, 1.9wt%, 2wt%, or the like.
Preferably, the refining in step (4) comprises any one or a combination of at least two of rectification, activated carbon adsorption or aeration.
Preferably, the rectification in the refining comprises extractive rectification.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) Rectifying the isopropanol waste liquid with the mass percent of 10-40wt% of isopropanol to obtain isopropanol pretreatment mother liquor and first crude isopropanol with the mass percent of 55-65wt% of isopropanol;
(2) The isopropanol pretreatment mother liquor in the step (1) is adsorbed by macroporous resin with the aperture of 100-1000 nm to obtain adsorption effluent; the mass percentage of the isopropanol in the isopropanol pretreatment mother liquor is 0.5-1%, and the chemical oxygen demand is 4000-10000 mg/L; the adsorption temperature is 5-45 ℃, and the flow of the isopropanol pretreatment mother liquor is 0.5-2 BV/h;
(3) Performing solvent regeneration on the resin adsorbed in the step (2) by using the first crude isopropanol in the step (1) to obtain second crude isopropanol; the regeneration temperature of the solvent is 5-45 ℃, the flow of the first crude isopropanol is 0.5-2 BV/h, and the dosage of the first crude isopropanol is 0.5-3 times of the volume of the resin;
the resin after the solvent regeneration is recycled to the step (2) for resin adsorption after the steam regeneration; the temperature of steam regeneration is 120-180 ℃, the mass of steam is 2-4 kg, and the pressure is 0.2-0.4 kPa;
mixing the steam condensate water after steam regeneration with the isopropanol waste liquid in the step (1), wherein the mass percentage of isopropanol in the steam condensate water is 1-2wt%;
(4) And refining the first crude isopropanol and the second crude isopropanol to obtain an isopropanol product.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) The method for regenerating the resin in the process for recovering the isopropanol provided by the invention adopts the first crude isopropanol to regenerate the resin, so that the aim of effectively regenerating the resin can be fulfilled, and the method is a mode of treating waste by waste;
(2) According to the method for recycling the resin in the isopropanol process, provided by the invention, after the solvent is recycled, the steam is used for deep recycling of the resin, so that the effects of cleaning residual isopropanol and deep recycling can be achieved, a small amount of steam condensate water can return to the isopropanol waste liquid, and secondary waste is not generated;
(3) The method for recovering the isopropanol from the isopropanol waste liquid improves the recycling frequency of the resin by improving the regeneration mode of the resin, and the resin can still have a better adsorption effect after at least 5 regeneration cycles, so that the cost for refining the isopropanol is reduced.
Drawings
FIG. 1 is a schematic flow chart of the method for recovering isopropanol from isopropanol waste liquid.
Detailed Description
The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings.
The present invention will be described in further detail below. The following examples are merely illustrative of the present invention and are not intended to represent or limit the scope of the invention as defined in the claims.
The flow chart of the method for recovering isopropanol from isopropanol waste liquid provided by the invention is shown in figure 1, and the method comprises the following steps:
(1) Rectifying the isopropanol waste liquid to obtain isopropanol pretreatment mother liquor and first crude isopropanol with the mass percent of isopropanol of 55-65wt%;
(2) The isopropanol pretreatment mother liquor in the step (1) is adsorbed by resin to obtain adsorption effluent;
(3) Performing solvent regeneration on the resin adsorbed in the step (2) by using the first crude isopropanol in the step (1) to obtain second crude isopropanol;
the resin after the solvent regeneration is recycled to the step (2) for resin adsorption after the steam regeneration;
mixing the steam condensate water after steam regeneration with the isopropanol waste liquid in the step (1);
(4) And refining the first crude isopropanol and the second crude isopropanol to obtain an isopropanol product.
1. Examples
Example 1
The embodiment provides a method for regenerating resin in an isopropanol recovery process, which comprises the following steps:
(A) Carrying out solvent regeneration on the adsorbed macroporous resin (the column height of the XDA experimental column is 30cm, the density of the macroporous resin is 1.2 g/mL) by utilizing the pretreated first crude isopropanol, wherein the temperature of the solvent regeneration is 40 ℃, the flow rate of the first crude isopropanol is 1BV/h, and the dosage of the first crude isopropanol is 2 times of the volume of the resin; the mass percentage of the isopropanol in the first crude isopropanol is 60wt%;
(B) And (3) carrying out steam regeneration on the macroporous resin subjected to the solvent regeneration in the step (A), wherein the steam regeneration temperature is 130 ℃, the steam mass is 3kg, and the pressure is 0.3kPa.
Example 2
The embodiment provides a method for regenerating resin in an isopropanol recovery process, which comprises the following steps:
(A) Carrying out solvent regeneration on the adsorbed macroporous resin (the column height of the XDA experimental column is 32cm, the density of the macroporous resin is 1.2 g/mL) by utilizing the pretreated first crude isopropanol, wherein the temperature of the solvent regeneration is 5 ℃, the flow rate of the first crude isopropanol is 0.5BV/h, and the dosage of the first crude isopropanol is 3 times of the volume of the resin;
(B) And (3) carrying out steam regeneration on the macroporous resin subjected to the solvent regeneration in the step (A), wherein the steam regeneration temperature is 180 ℃, the steam mass is 4kg, and the pressure is 0.4kPa.
Example 3
The embodiment provides a method for regenerating resin in an isopropanol recovery process, which comprises the following steps:
(A) Carrying out solvent regeneration on the adsorbed macroporous resin (the column height of the XDA experimental column is 28cm, the density of the macroporous resin is 1.2 g/mL) by utilizing the pretreated first crude isopropanol, wherein the temperature of the solvent regeneration is 45 ℃, the flow rate of the first crude isopropanol is 2BV/h, and the dosage of the first crude isopropanol is 0.5 times of the volume of the resin;
(B) And (3) carrying out steam regeneration on the macroporous resin subjected to the solvent regeneration in the step (A), wherein the steam regeneration temperature is 120 ℃, the steam mass is 2kg, and the pressure is 0.2kPa.
Example 4
The embodiment provides a method for recovering isopropanol from isopropanol waste liquid, which comprises the following steps:
(1) Rectifying the isopropanol waste liquid with the mass percent of the isopropanol of 20wt% to obtain isopropanol pretreatment mother liquor and first crude isopropanol with the mass percent of the isopropanol of 55 wt%;
(2) The isopropanol pretreatment mother liquor is adsorbed by macroporous resin with the aperture of 500nm (the column height of an XDA experimental column is 30cm, and the density of the macroporous resin is 1.2 g/mL), so as to obtain adsorption effluent; the mass percentage of the isopropanol in the isopropanol pretreatment mother liquor is 0.8%, and the chemical oxygen demand is 4574mg/L; the adsorption temperature is 25 ℃, and the flow of the isopropanol pretreatment mother liquor is 1BV/h;
(3) Performing solvent regeneration on the macroporous resin adsorbed in the step (2) by using the first crude isopropanol in the step (1) to obtain second crude isopropanol; the temperature of the solvent regeneration is 25 ℃, the flow of the first crude isopropanol is 1BV/h, and the dosage of the first crude isopropanol is 1.2 times of the volume of the resin;
the macroporous resin after solvent regeneration is recycled to the step (2) for resin adsorption after steam regeneration; the temperature of steam regeneration is 150 ℃, the mass of steam is 3kg, and the pressure is 0.3kPa;
mixing the steam condensate water after steam regeneration with the isopropanol waste liquid in the step (1), wherein the mass percentage of isopropanol in the steam condensate water is 1.5wt%;
(4) And refining the first crude isopropanol and the second crude isopropanol to obtain an isopropanol product.
Example 5
The embodiment provides a method for recovering isopropanol from isopropanol waste liquid, which comprises the following steps:
(1) Rectifying the isopropanol waste liquid with the mass percent of 10wt% of isopropanol to obtain isopropanol pretreatment mother liquor and first crude isopropanol with the mass percent of 55wt% of isopropanol;
(2) The isopropanol pretreatment mother liquor is adsorbed by macroporous resin with the aperture of 100nm (the column height of an XDA experimental column is 32cm, and the density of the macroporous resin is 1.2 g/mL), so as to obtain adsorption effluent; the mass percentage of the isopropanol in the isopropanol pretreatment mother liquor is 0.5%, and the chemical oxygen demand is 4000mg/L; the adsorption temperature is 5 ℃, and the flow of the isopropanol pretreatment mother liquor is 0.5BV/h;
(3) Performing solvent regeneration on the macroporous resin adsorbed in the step (2) by using the first crude isopropanol in the step (1) to obtain second crude isopropanol; the temperature of the solvent regeneration is 5 ℃, the flow of the first crude isopropanol is 0.5BV/h, and the dosage of the first crude isopropanol is 0.5 times of the volume of the resin;
the macroporous resin after solvent regeneration is recycled to the step (2) for resin adsorption after steam regeneration; the temperature of steam regeneration is 120 ℃, the mass of steam is 2kg, and the pressure is 0.2kPa;
mixing the steam condensate water after steam regeneration with the isopropanol waste liquid in the step (1), wherein the mass percentage of isopropanol in the steam condensate water is 1wt%;
(4) And refining the first crude isopropanol and the second crude isopropanol to obtain a refined isopropanol product.
Example 6
The embodiment provides a method for recovering isopropanol from isopropanol waste liquid, which comprises the following steps:
(1) Rectifying the isopropanol waste liquid with the mass percent of the isopropanol of 40 percent to obtain isopropanol pretreatment mother liquor and first crude isopropanol with the mass percent of the isopropanol of 65 percent;
(2) The isopropanol pretreatment mother liquor is adsorbed by macroporous resin with the aperture of 1000nm (the column height of an XDA experimental column is 32cm, and the density of the macroporous resin is 1.2 g/mL), so as to obtain adsorption effluent; the mass percentage of the isopropanol in the isopropanol pretreatment mother liquor is 1%, and the chemical oxygen demand is 10000mg/L; the adsorption temperature is 45 ℃, and the flow of the isopropanol pretreatment mother liquor is 2BV/h;
(3) Performing solvent regeneration on the macroporous resin adsorbed in the step (2) by using the first crude isopropanol in the step (1) to obtain second crude isopropanol; the temperature of the solvent regeneration is 45 ℃, the flow of the first crude isopropanol is 2BV/h, and the dosage of the first crude isopropanol is 3 times of the volume of the resin;
the macroporous resin after solvent regeneration is recycled to the step (2) for resin adsorption after steam regeneration; the temperature of steam regeneration is 180 ℃, the mass of steam is 4kg, and the pressure is 0.4kPa;
mixing the steam condensate water after steam regeneration with the isopropanol waste liquid in the step (1), wherein the mass percentage of isopropanol in the steam condensate water is 2 percent;
(4) And refining the first crude isopropanol and the second crude isopropanol to obtain an isopropanol product.
Example 7
This example provides a process for recovering isopropanol from an isopropanol waste stream, which is the same as in example 4 except that the steam regeneration temperature in step (3) is 100 ℃.
Example 8
This example provides a process for recovering isopropanol from an isopropanol waste stream, the process being the same as in example 4 except that the steam regeneration temperature in step (3) is 200 ℃.
Example 9
This example provides a process for recovering isopropanol from an isopropanol effluent, which is the same as example 4 except that the flow rate of the first crude isopropanol in the solvent regeneration of step (3) is 0.2 BV/h.
Example 10
This example provides a process for recovering isopropanol from an isopropanol effluent, which is the same as example 4 except that the flow rate of the first crude isopropanol in the solvent regeneration of step (3) is 2.5 BV/h.
2. Comparative example
Comparative example 1
This comparative example provides a method for recovering isopropyl alcohol from isopropyl alcohol waste liquid, which is the same as in example 4 except that in step (3), solvent regeneration is not performed, and only steam regeneration is performed.
Comparative example 2
This comparative example provides a method for recovering isopropyl alcohol from isopropyl alcohol waste liquid, which is the same as in example 4 except that only solvent regeneration is performed in step (3) and steam regeneration is not performed.
3. Testing and results
Taking example 4 as an example, 5L of isopropanol waste liquid is rectified to obtain 2L of first crude isopropanol and 3L of isopropanol pre-rectification mother liquor, and the COD (chemical oxygen demand) detection is carried out on adsorption effluent adsorbed by the isopropanol pre-rectification mother liquor by using a dichromate method in the measurement of HJ 828-2017-water quality-chemical oxygen demand, wherein each 200mL of adsorption effluent is sampled.
TABLE 1
| Number of samplings | COD/mg·L -1 |
| Isopropyl alcohol pretreatment mother liquor | 4574 |
| 1(200mL) | 391 |
| 2(200mL) | 376 |
| 3(200mL) | 411 |
| 4(200mL) | 480 |
| 5(200mL) | 490 |
| 6(200mL) | 560 |
| 7(200mL) | 1180 |
| 8(200mL) | 2380 |
| 9(200mL) | 3900 |
As can be seen from Table 1, the method provided by the invention has a good adsorption effect on organic matters in the isopropanol treatment mother liquor, and the COD value content in the effluent after adsorption is 4574 mg.L -1 Reduced to 391 mg.L -1 The treatment effect is good.
The resin was regenerated by the regeneration method provided in example 4, examples 7 to 10 and comparative examples 1 to 2 and recycled 8 times, and the COD of the adsorbed effluent from the sixth sampling of the resin was detected by the dichromate method in the measurement of HJ 828-2017-water quality-chemical oxygen demand, and the results are shown in Table 2.
TABLE 2
From table 2, the following points can be seen:
(1) It can be seen from comprehensive examples 4-10 that the resin regeneration method in the method for recovering isopropanol from isopropanol waste liquid provided by the invention can realize effective regeneration of resin, and the resin still maintains better adsorption performance after at least 5 times of regeneration, thereby reducing the cost of refining isopropanol;
(2) As can be seen from the combination of examples 4 and examples 7 to 8, the steam regeneration temperature in example 4 was 130℃and the effect of the cycle regeneration 8 times in example 4 on the use of the resin was less than the steam regeneration temperatures in examples 7 and 8 of 100℃and 200℃respectively, whereas the COD value of the adsorbed effluent water was not less than 800/mg.L when the cycle was used 6 times due to the accumulation of organics in the resin due to the lower regeneration temperature after 5 times of the cycle use in example 7 -1 While in example 8, although the steam regeneration temperature is increased, the improvement on the cycle performance is small and the energy consumption is high, so that the invention is shown that the steam regeneration temperature is preferably controlled in a specific range, thereby ensuring the steam regeneration effect and saving the energy consumption;
(3) As can be seen from the comprehensive examples 4 and comparative examples 1 to 2, in example 4, the solvent regeneration is performed by using crude isopropanol, and then the steam regeneration is performed, and compared with the comparative examples 1 and 2, which use only steam regeneration and solvent regeneration respectively, the regenerated resin has poor adsorption effect, so that the invention has the effect of cooperatively regenerating the resin by using the crude isopropanol solvent regeneration and the combined steam regeneration, and the service life of the resin is prolonged.
In summary, the method for regenerating resin in the process for recovering isopropanol provided by the invention firstly regenerates the resin by adopting the first crude isopropanol, simultaneously achieves the purposes of effectively regenerating the resin and treating waste by waste, and then uses steam for regeneration to play roles of cleaning residual isopropanol and deeply regenerating, so that the resin has long cycle service life, has good adsorption effect after at least 5 regeneration cycles, and reduces the cost of the process for recovering isopropanol.
The applicant states that the detailed structural features of the present invention are described by the above embodiments, but the present invention is not limited to the above detailed structural features, i.e. it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.
Claims (21)
1. A method for recovering isopropyl alcohol from isopropyl alcohol waste liquid, the method comprising the steps of:
(1) Pretreating the isopropanol waste liquid to obtain isopropanol pretreatment mother liquor and first crude isopropanol;
(2) The isopropanol pretreatment mother liquor in the step (1) is adsorbed by resin to obtain adsorption effluent;
(3) Performing solvent regeneration on the resin adsorbed in the step (2) by using the first crude isopropanol in the step (1) to obtain second crude isopropanol;
the resin after the solvent regeneration is recycled to the step (2) for resin adsorption after the steam regeneration;
(4) And refining the first crude isopropanol and the second crude isopropanol to obtain an isopropanol product.
2. The method according to claim 1, wherein the mass percentage of isopropanol in the first crude isopropanol is 55-65 wt%.
3. The method of claim 1, wherein the resin comprises a macroporous resin.
4. The method according to claim 1, wherein the temperature of the solvent regeneration is 5-45 ℃.
5. The process according to claim 1, wherein the flow rate of the first crude isopropyl alcohol in the solvent regeneration is 0.5-2 BV/h.
6. The method according to claim 1, wherein the amount of the first crude isopropyl alcohol used in the solvent regeneration is 0.5 to 3 times the volume of the resin.
7. The method according to claim 1 or 2, wherein the temperature of steam regeneration is 120-180 ℃.
8. A method according to claim 1 or 2, characterized in that the mass of steam in the steam regeneration is 2-4 kg.
9. The method of claim 7, wherein the pressure of steam regeneration is 0.2 to 0.4kPa.
10. The method according to claim 1, wherein the mass percentage of the isopropanol in the isopropanol waste liquid in the step (1) is 10-40 wt%.
11. The method of claim 1, wherein the pretreatment in step (1) comprises rectification.
12. A method according to claim 3, wherein the macroporous resin has a pore size of 100 to 1000nm.
13. The method according to claim 1, wherein the isopropanol pretreatment mother liquor contains 0.5-1% by mass of isopropanol.
14. The method according to claim 13, wherein the chemical oxygen demand in the isopropyl alcohol pretreatment mother liquor is 4000 to 10000mg/L.
15. The method of claim 1, wherein the adsorbed effluent has a chemical oxygen demand of < 500mg/L.
16. The method according to claim 1, wherein the temperature of the adsorption in step (2) is 5 to 45 ℃.
17. The method according to claim 1, wherein the flow rate of the isopropanol pretreatment mother liquor in the adsorption is 0.5-2 BV/h.
18. The method according to claim 1, wherein the steam condensate regenerated in step (3) is mixed with the isopropyl alcohol waste liquid in step (1).
19. The method according to claim 18, wherein the mass percentage of isopropanol in the steam condensate is 1-2 wt%.
20. The method of claim 1, wherein the refining in step (4) comprises a refining process of any one or a combination of at least two of rectification, activated carbon adsorption, or aeration.
21. The method of claim 20, wherein the rectification in the refining comprises extractive distillation.
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| US4147624A (en) * | 1976-04-15 | 1979-04-03 | Arthur D. Little, Inc. | Wastewater treatment with desorbing of an adsorbate from an adsorbent with a solvent in the near critical state |
| JPS63236504A (en) * | 1987-03-24 | 1988-10-03 | Ube Ind Ltd | Regenerating method for adsorption tower |
| US5104545A (en) * | 1989-12-15 | 1992-04-14 | Nalco Chemical Company | Process for removing water soluble organic compounds from produced water |
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| CN105174577A (en) * | 2015-08-06 | 2015-12-23 | 中钢集团鞍山热能研究院有限公司 | Coal chemical wastewater pretreatment process and device |
| CN107253901A (en) * | 2017-07-26 | 2017-10-17 | 四川天采科技有限责任公司 | A kind of separation of high-purity isopropanol and purification method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR3004442B1 (en) * | 2013-04-10 | 2017-05-05 | Veolia Water Solutions & Tech | METHOD AND INSTALLATION FOR TREATING WATER FROM OIL AND GAS INDUSTRIES, IN PARTICULAR PRODUCING WATER FROM PETROLEUM AND / OR GAS FIELDS. |
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| US4147624A (en) * | 1976-04-15 | 1979-04-03 | Arthur D. Little, Inc. | Wastewater treatment with desorbing of an adsorbate from an adsorbent with a solvent in the near critical state |
| JPS63236504A (en) * | 1987-03-24 | 1988-10-03 | Ube Ind Ltd | Regenerating method for adsorption tower |
| US5104545A (en) * | 1989-12-15 | 1992-04-14 | Nalco Chemical Company | Process for removing water soluble organic compounds from produced water |
| CN102942447A (en) * | 2012-10-13 | 2013-02-27 | 江苏盈天化学有限公司 | Purification method for electronic grade isopropanol recovered liquid |
| CN105174577A (en) * | 2015-08-06 | 2015-12-23 | 中钢集团鞍山热能研究院有限公司 | Coal chemical wastewater pretreatment process and device |
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