CN112044419A - Method for regenerating resin in isopropanol recovery process - Google Patents

Method for regenerating resin in isopropanol recovery process Download PDF

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CN112044419A
CN112044419A CN202010871521.XA CN202010871521A CN112044419A CN 112044419 A CN112044419 A CN 112044419A CN 202010871521 A CN202010871521 A CN 202010871521A CN 112044419 A CN112044419 A CN 112044419A
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isopropanol
resin
regeneration
steam
crude
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CN112044419B (en
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伍元东
孙志洋
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WUXI ZHONGTIAN SOLID WASTE DISPOSAL CO Ltd
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WUXI ZHONGTIAN SOLID WASTE DISPOSAL CO Ltd
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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
    • 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
    • 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
    • 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: carrying out solvent regeneration on the adsorbed resin by utilizing the pretreated first crude isopropanol; and the steam is adopted to carry out steam regeneration on the resin after the solvent regeneration, wherein the first crude isopropanol regenerates the resin, and simultaneously, the purposes of effectively regenerating the resin and treating wastes with wastes are achieved, and the effects of cleaning residual isopropanol and deeply regenerating are achieved by using the steam regeneration, so that the resin has long cycle service life, and the cost of the isopropanol recovery process is reduced.

Description

Method for regenerating resin in isopropanol recovery process
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
Isopropanol is an organic compound, namely isomer of n-propanol, namely dimethyl methanol and 2-propanol, is also called IPA in the industry, is colorless transparent liquid, has the smell similar to the mixture of ethanol and acetone, is dissolved in water, is also dissolved in most organic solvents such as alcohol, ether, benzene, chloroform and the like, and is an important chemical product and raw material.
At present, in the electronic industry or the printing industry, isopropanol is commonly used as 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 post-treatment of wastewater is difficult.
CN2539738Y discloses an apparatus for extracting isopropanol from waste liquid of cleaning printing plates, and CN1249294A discloses a method for refining isopropanol by salt extraction and azeotropic distillation combined process, wherein the method uses a rectification mode to recover high-purity isopropanol, but does not mention how to dispose isopropanol mother liquid.
CN102173521B discloses a treatment method of high-concentration industrial wastewater containing isopropanol, which uses a catalytic oxidation method to treat isopropanol wastewater, but because isopropanol is easy to volatilize, an aeration mode can generate isopropanol waste gas to cause secondary pollution.
CN104525114B discloses a method for treating isopropanol wastewater by using modified activated carbon to adsorb the isopropanol wastewater, but the initial COD value capable of being treated is low, and the activated carbon needs high-temperature regeneration and has high requirements on equipment.
Therefore, it is highly desirable to develop a method for recovering isopropanol to achieve the purpose of reducing the cost and emission.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a method for regenerating resin in an isopropanol recovery process, which regenerates the resin by using first crude isopropanol, simultaneously achieves the purposes of effectively regenerating the resin and treating wastes with wastes, and plays roles in cleaning residual isopropanol and deeply regenerating by using steam regeneration, so that the resin has long cycle service life, and the cost of the isopropanol recovery process is reduced.
In order 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 a process for recovering isopropanol, the method comprising: carrying out solvent regeneration on the adsorbed resin by utilizing the pretreated first crude isopropanol; and then the 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 wastes with wastes are achieved, and the effects of cleaning residual isopropanol and deeply regenerating are achieved by using steam regeneration, so that the recycling service life of the resin is prolonged compared with pure steam regeneration; compared with pure solvent regeneration, the regeneration cost is reduced, the problem of regenerated solvent treatment does not exist, and the method has higher economic benefit and environmental protection benefit.
Preferably, the isopropanol in the first crude isopropanol is 55-65 wt%, for example, 55 wt%, 56 wt%, 57 wt%, 58 wt%, 59 wt%, 60 wt%, 61 wt%, 62 wt%, 63 wt%, 64 wt% or 65 wt%.
Preferably, the resin comprises a macroporous resin.
Preferably, the temperature for solvent regeneration is 5-45 ℃, for example, can be 5 ℃, 10 ℃, 12 ℃, 15 ℃, 18 ℃, 20 ℃, 22 ℃, 25 ℃, 28 ℃, 30 ℃, 35 ℃, 40 ℃ or 45 ℃.
Preferably, the flow rate of the first crude isopropanol in the solvent regeneration is 0.5-2 BV/h, 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 or 2BV/h, etc.
Preferably, the amount of the first crude isopropanol used in the solvent regeneration is 0.5 to 3 times of the volume of the resin, 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, or 3 times.
Preferably, the temperature of the steam regeneration is 120 to 180 ℃, for example, 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 160 ℃, 165 ℃, 170 ℃, 175 ℃ or 180 ℃ and the like.
The method strictly controls the temperature of steam regeneration 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 4 kg.
Preferably, the pressure of the steam regeneration is 0.2 to 0.4kPa, and may be, for example, 0.2kPa, 0.22kPa, 0.25kPa, 0.26kPa, 0.28kPa, 0.3kPa, 0.32kPa, 0.35kPa, 0.38kPa, or 0.4 kPa.
As a preferred technical solution of the present invention, the method comprises: carrying out solvent regeneration on the adsorbed resin by utilizing the pretreated first crude isopropanol; carrying out steam regeneration on the resin after the solvent regeneration by adopting steam; the regeneration temperature of the solvent is 5-45 ℃, the flow rate 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 the steam regeneration is 120-180 ℃, the mass of the steam is 2-4 kg, and the pressure is 0.2-0.4 kPa.
In a second aspect, the invention provides a method for recovering isopropanol from an isopropanol waste liquid, wherein the method adopts the method for regenerating resin in the isopropanol recovery process of the first aspect to regenerate resin.
The method for recovering the isopropanol from the isopropanol waste liquid provided by the invention 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 liquid and first crude isopropanol;
(2) adsorbing the isopropanol pretreatment mother liquor obtained in the step (1) by resin to obtain adsorbed effluent;
(3) carrying out 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 being subjected to steam regeneration;
(4) and refining the first crude isopropanol and the second crude isopropanol to obtain isopropanol products.
Preferably, the content of isopropanol in the isopropanol waste liquid in the step (1) is 10-40 wt%, for example, 10 wt%, 12 wt%, 15 wt%, 18 wt%, 20 wt%, 22 wt%, 25 wt%, 28 wt%, 30 wt%, 32 wt%, 33 wt%, 35 wt%, 38 wt% or 40 wt%.
The isopropanol waste liquid provided by the invention mainly contains water, the isopropanol content is 10-40 wt%, and 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 a production process thereof.
Preferably, the pretreatment in step (1) comprises rectification.
The distillation is not particularly limited by the present invention and may be carried out by distillation capable of preliminary separation of water and isopropanol well known to those skilled in the art.
Preferably, the isopropanol in the first crude isopropanol is 55-65 wt%, for example, 55 wt%, 56 wt%, 57 wt%, 58 wt%, 59 wt%, 60 wt%, 61 wt%, 62 wt%, 63 wt%, 64 wt% or 65 wt%.
Preferably, the resin in step (2) comprises a macroporous resin.
Preferably, the pore diameter of the macroporous resin is 100-1000 nm, and may be, for example, 100nm, 200nm, 300nm, 400nm, 500nm, 600nm, 700nm, 800nm, 900nm, 1000nm, or the like.
Preferably, the content of isopropanol in the isopropanol pretreatment mother liquor is 0.5-1% by mass, and may be, 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 or 10000 mg/L.
Preferably, the adsorbed water has a chemical oxygen demand of < 500mg/L, such as 499mg/L, 495mg/L, 490mg/L, 470mg/L, 450mg/L, 440mg/L, 400mg/L, 380mg/L, 350mg/L or 300 mg/L.
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 ℃ or 45 ℃.
Preferably, the flow rate of the isopropanol pretreatment mother liquor in the adsorption is 0.5-2 BV/h, and can be 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 and the like.
Preferably, the steam condensate water after the steam regeneration in the step (3) is mixed with the isopropanol waste liquid in the step (1) for treatment.
Preferably, the content of the isopropanol in the steam condensate water is 1-2 wt%, for example, 1 wt%, 1.1 wt%, 1.2 wt%, 1.3 wt%, 1.4 wt%, 1.5 wt%, 1.6 wt%, 1.7 wt%, 1.8 wt%, 1.9 wt%, 2 wt%, etc.
Preferably, the refining in the step (4) comprises a refining method of 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 isopropanol of 10-40 wt% to obtain isopropanol pretreatment mother liquid and first crude isopropanol with the mass percent of isopropanol of 55-65 wt%;
(2) adsorbing the isopropanol pretreatment mother liquor obtained in the step (1) by macroporous resin with the aperture of 100-1000 nm to obtain adsorbed 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) carrying out 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 rate 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 being subjected to steam regeneration; the temperature of the steam regeneration is 120-180 ℃, the mass of the steam is 2-4 kg, and the pressure is 0.2-0.4 kPa;
mixing the steam condensate after the steam regeneration with the isopropanol waste liquid obtained in the step (1), wherein the mass percentage of the isopropanol in the steam condensate is 1-2 wt%;
(4) and refining the first crude isopropanol and the second crude isopropanol to obtain isopropanol products.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the method for regenerating the resin in the isopropanol recovery process provided by the invention adopts the first crude isopropanol to regenerate the resin, so that the aim of effectively regenerating the resin can be achieved, and a mode of treating waste by waste is realized;
(2) according to the method for resin regeneration in the isopropanol recovery process, provided by the invention, after the solvent is regenerated, the steam regeneration is used for deeply regenerating the resin, so that residual isopropanol can be cleaned and deeply regenerated, a small amount of steam condensate water can be returned 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 times of the resin by improving the resin regeneration mode, and the resin still has better adsorption effect after at least 5 regeneration cycles, thereby reducing the cost of refining the isopropanol.
Drawings
FIG. 1 is a schematic flow diagram of a method for recovering isopropanol from an isopropanol waste liquid provided by the present invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
The flow schematic diagram 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 percentage of the isopropanol of 55-65 wt%;
(2) adsorbing the isopropanol pretreatment mother liquor obtained in the step (1) by resin to obtain adsorbed effluent;
(3) carrying out 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 being subjected to steam regeneration;
mixing the steam condensate water after the 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 isopropanol products.
First, an embodiment
Example 1
This example provides a method for resin regeneration in a process for recovering isopropanol, the method comprising the steps of:
(A) carrying out solvent regeneration on the adsorbed macroporous resin (the column height of an XDA experimental column is 30cm, and the density of the macroporous resin is 1.2g/mL) by utilizing the pretreated first crude isopropanol, wherein the temperature for solvent regeneration is 40 ℃, the flow rate of the first crude isopropanol is 1BV/h, and the using amount 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 60 wt%;
(B) and (3) carrying out steam regeneration on the macroporous resin subjected to solvent regeneration in the step (A) by adopting steam, wherein the steam regeneration temperature is 130 ℃, the steam quality is 3kg, and the pressure is 0.3 kPa.
Example 2
This example provides a method for resin regeneration in a process for recovering isopropanol, the method comprising the steps of:
(A) carrying out solvent regeneration on the adsorbed macroporous resin (the column height of an XDA experimental column is 32cm, and the density of the macroporous resin is 1.2g/mL) by utilizing the pretreated first crude isopropanol, wherein the temperature for solvent regeneration is 5 ℃, the flow rate of the first crude isopropanol is 0.5BV/h, and the using amount 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 solvent regeneration in the step (A) by adopting steam, wherein the steam regeneration temperature is 180 ℃, the steam quality is 4kg, and the pressure is 0.4 kPa.
Example 3
This example provides a method for resin regeneration in a process for recovering isopropanol, the method comprising the steps of:
(A) carrying out solvent regeneration on the adsorbed macroporous resin (the column height of an XDA experimental column is 28cm, and the density of the macroporous resin is 1.2g/mL) by utilizing the pretreated first crude isopropanol, wherein the temperature for solvent regeneration is 45 ℃, the flow rate of the first crude isopropanol is 2BV/h, and the using amount 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 solvent regeneration in the step (A) by adopting steam, wherein the steam regeneration temperature is 120 ℃, the steam quality is 2kg, and the pressure is 0.2 kPa.
Example 4
The embodiment provides a method for recovering isopropanol from an isopropanol waste liquid, which comprises the following steps:
(1) rectifying the isopropanol waste liquid with the mass percent of isopropanol of 20 wt% to obtain isopropanol pretreatment mother liquor and first crude isopropanol with the mass percent of isopropanol of 55 wt%;
(2) adsorbing the isopropanol pretreated mother liquor in the step (1) by macroporous resin with the aperture of 500nm (the column height of an XDA experimental packed column is 30cm, and the density of the macroporous resin is 1.2g/mL) to obtain adsorbed effluent; the mass percentage of the isopropanol in the isopropanol pretreatment mother liquor is 0.8%, and the chemical oxygen demand is 4574 mg/L; the adsorption temperature is 25 ℃, and the flow of the isopropanol pretreatment mother liquor is 1 BV/h;
(3) carrying out 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 regeneration temperature of the solvent is 25 ℃, the flow rate of the first crude isopropanol is 1BV/h, and the using amount of the first crude isopropanol is 1.2 times of the volume of the resin;
the macroporous resin after the solvent regeneration is recycled to the step (2) for resin adsorption after being subjected to steam regeneration; the temperature of the steam regeneration is 150 ℃, the mass of the steam is 3kg, and the pressure is 0.3 kPa;
mixing the steam condensate after the steam regeneration with the isopropanol waste liquid in the step (1), wherein the mass percentage of the isopropanol in the steam condensate is 1.5 wt%;
(4) and refining the first crude isopropanol and the second crude isopropanol to obtain isopropanol products.
Example 5
The embodiment provides a method for recovering isopropanol from an isopropanol waste liquid, which comprises the following steps:
(1) rectifying the isopropanol waste liquid with the mass percent of isopropanol of 10 wt% to obtain isopropanol pretreatment mother liquor and first crude isopropanol with the mass percent of isopropanol of 55 wt%;
(2) adsorbing the isopropanol pretreated mother liquor in the step (1) by macroporous resin with the aperture of 100nm (the column height of an XDA experimental packed column is 32cm, and the density of the macroporous resin is 1.2g/mL) to obtain adsorbed effluent; the mass percentage of the isopropanol in the isopropanol pretreatment mother liquor is 0.5%, and the chemical oxygen demand is 4000 mg/L; the adsorption temperature is 5 ℃, and the flow rate of the isopropanol pretreatment mother liquor is 0.5 BV/h;
(3) carrying out 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 regeneration temperature of the solvent is 5 ℃, the flow rate of the first crude isopropanol is 0.5BV/h, and the using amount of the first crude isopropanol is 0.5 times of the volume of the resin;
the macroporous resin after the solvent regeneration is recycled to the step (2) for resin adsorption after being subjected to steam regeneration; the temperature of the steam regeneration is 120 ℃, the mass of the steam is 2kg, and the pressure is 0.2 kPa;
mixing the steam condensate after the steam regeneration with the isopropanol waste liquid in the step (1), wherein the mass percentage of the isopropanol in the steam condensate is 1 wt%;
(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 an isopropanol waste liquid, which comprises the following steps:
(1) rectifying the isopropanol waste liquid with the mass percent of isopropanol of 40 wt% to obtain isopropanol pretreatment mother liquor and first crude isopropanol with the mass percent of isopropanol of 65 wt%;
(2) adsorbing the isopropanol pretreatment mother liquor in the step (1) by macroporous resin with the aperture of 1000nm (the column height of an XDA experimental packed column is 32cm, and the density of the macroporous resin is 1.2g/mL) to obtain adsorbed effluent; the mass percentage of the isopropanol in the isopropanol pretreatment mother liquor is 1%, and the chemical oxygen demand is 10000 mg/L; the adsorption temperature is 45 ℃, and the flow rate of isopropanol pretreatment mother liquor is 2 BV/h;
(3) carrying out 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 regeneration temperature of the solvent is 45 ℃, the flow rate of the first crude isopropanol is 2BV/h, and the using amount of the first crude isopropanol is 3 times of the volume of the resin;
the macroporous resin after the solvent regeneration is recycled to the step (2) for resin adsorption after being subjected to steam regeneration; the temperature of the steam regeneration is 180 ℃, the mass of the steam is 4kg, and the pressure is 0.4 kPa;
mixing the steam condensate after the steam regeneration with the isopropanol waste liquid in the step (1), wherein the mass percentage of the isopropanol in the steam condensate is 2 wt%;
(4) and refining the first crude isopropanol and the second crude isopropanol to obtain isopropanol products.
Example 7
This example provides a process for recovering isopropanol from an isopropanol waste liquid, which is the same as in example 4 except that the temperature of steam regeneration in step (3) is 100 ℃.
Example 8
This example provides a process for recovering isopropanol from an isopropanol waste liquid, which is the same as in example 4 except that the temperature of steam regeneration in step (3) is 200 ℃.
Example 9
This example provides a process for recovering isopropanol from an isopropanol waste liquid, which is the same as in 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 waste liquid, which is the same as in example 4 except that the flow rate of the first crude isopropanol in the solvent regeneration of step (3) is 2.5 BV/h.
Second, comparative example
Comparative example 1
This comparative example provides a process for recovering isopropanol from an isopropanol waste liquid, which is the same as in example 4 except that in step (3), the solvent regeneration is not performed, and only the steam regeneration is performed.
Comparative example 2
This comparative example provides a process for recovering isopropanol from an isopropanol waste liquid, which is the same as in example 4 except that only solvent regeneration is carried out in step (3) and steam regeneration is not carried out.
Third, test 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 liquid, and the adsorbed water adsorbed by the isopropanol pre-rectification mother liquid is subjected to COD detection by a dichromate method in the determination of HJ 828-.
TABLE 1
Number of samplings COD/mg·L-1
Mother liquor of isopropanol pretreatment 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 better 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-1Reduced to 391 mg. L-1And the treatment effect is good.
The regeneration methods provided in examples 4, 7-10 and 1-2 were used to regenerate the resin, and the resin was recycled for 8 times, and the adsorbed effluent of the sixth sampling of the resin was subjected to COD detection by the dichromate method in the measurement of HJ 828-.
TABLE 2
Figure BDA0002651272200000121
Figure BDA0002651272200000131
From table 2, the following points can be seen:
(1) it can be seen from the comprehensive examples 4 to 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, maintain good adsorption performance after at least 5 times of resin regeneration, and reduce the cost of refining isopropanol;
(2) it can be seen from the combination of example 4 and examples 7-8 that the temperature of steam regeneration in example 4 is 130 ℃, compared with the temperatures of steam regeneration in examples 7 and 8 of 100 ℃ and 200 ℃, respectively, the effect of cyclic regeneration 8 times on the use of resin in example 4 is less, and the regeneration temperature is lower after cyclic use for 5 times in example 7, the organic matter is accumulated in the resin, and the COD value of the adsorbed water is not less than 800/mg.L.when cyclic use is 6 times-1Although the steam regeneration temperature is increased in the embodiment 8, the improvement on the cycle performance is small, and the energy consumption is high, so that the invention preferably controls the steam regeneration temperature in a specific range, thereby not only ensuring the steam regeneration effect, but also saving the energy consumption;
(3) it can be seen from the comprehensive examples 4 and comparative examples 1-2 that in example 4, crude isopropanol is firstly used for solvent regeneration and then steam regeneration is performed, and compared with the method that only steam regeneration and solvent regeneration are respectively used in comparative example 1 and comparative example 2, the adsorption effect of the regenerated resin is poor, so that the method provided by the invention has the advantages that the effect of synergistically regenerating the resin is achieved by adopting a mode of combining crude isopropanol solvent regeneration with steam regeneration, and the service life of the resin is prolonged.
In summary, according to the method for regenerating the resin in the process for recovering the isopropanol, provided by the invention, the first crude isopropanol is firstly adopted to regenerate the resin, and meanwhile, the purposes of effectively regenerating the resin and treating wastes with wastes are achieved, the effects of cleaning the residual isopropanol and deeply regenerating are achieved by using steam regeneration, the resin has long cycle service life, the adsorption effect is good after at least 5 times of regeneration cycles, and the cost of the process for recovering the isopropanol is reduced.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (10)

1. A method for regenerating resin in a process for recovering isopropanol, the method comprising:
carrying out solvent regeneration on the adsorbed resin by utilizing the pretreated first crude isopropanol; and then the steam is adopted to carry out steam regeneration on the resin after the solvent regeneration.
2. The method according to claim 1, wherein the isopropanol in the first crude isopropanol accounts for 55-65 wt%;
preferably, the resin comprises a macroporous resin;
preferably, the temperature for regenerating the solvent is 5-45 ℃;
preferably, the flow rate of the first crude isopropanol in the solvent regeneration is 0.5-2 BV/h;
preferably, the dosage of the first crude isopropanol in the solvent regeneration is 0.5-3 times of the volume of the resin.
3. The method according to claim 1 or 2, wherein the temperature of the steam regeneration is 120-180 ℃;
preferably, the mass of the steam in the steam regeneration is 2-4 kg;
preferably, the pressure of the steam regeneration is 0.2-0.4 kPa.
4. A method for recovering isopropanol from an isopropanol waste liquid, which is characterized in that the method adopts the method for regenerating resin in the isopropanol recovery process of any claim 1-3 to regenerate the resin.
5. Method according to claim 4, characterized in that it comprises the following steps:
(1) pretreating the isopropanol waste liquid to obtain isopropanol pretreatment mother liquid and first crude isopropanol;
(2) adsorbing the isopropanol pretreatment mother liquor obtained in the step (1) by resin to obtain adsorbed effluent;
(3) carrying out 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 being subjected to steam regeneration;
(4) and refining the first crude isopropanol and the second crude isopropanol to obtain isopropanol products.
6. The method according to claim 5, characterized in that the mass percentage of the isopropanol in the isopropanol waste liquid in the step (1) is 10-40 wt%;
preferably, the pretreatment in step (1) comprises rectification;
preferably, the mass percentage of the isopropanol in the first crude isopropanol is 55-65 wt%.
7. The method of claim 5 or 6, wherein the resin in step (2) comprises a macroporous resin;
preferably, the pore diameter of the macroporous resin is 100-1000 nm;
preferably, the mass percentage of the isopropanol in the isopropanol pretreatment mother liquor is 0.5-1%;
preferably, the chemical oxygen demand in the isopropanol pretreatment mother liquor is 4000-10000 mg/L;
preferably, the adsorbed water has a chemical oxygen demand of < 500 mg/L.
8. The method according to any one of claims 5 to 7, wherein the temperature of the adsorption in the step (2) is 5 to 45 ℃;
preferably, the flow rate of the isopropanol pretreatment mother liquor in the adsorption is 0.5-2 BV/h.
9. The method according to any one of claims 5 to 8, characterized in that steam condensate water after the steam regeneration in the step (3) is mixed with isopropanol waste liquid in the step (1) for treatment;
preferably, the mass percentage of the isopropanol in the steam condensate water is 1-2 wt%.
10. The method according to any one of claims 5 to 9, wherein the refining in the step (4) comprises a refining method of 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.
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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
US20160075581A1 (en) * 2013-04-10 2016-03-17 Veolia Water Solutions & Technologies Support Method and installation for treating water coming from the petroleum and gas industries, especially production water from petroleum and/or gas fields
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

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
US20160075581A1 (en) * 2013-04-10 2016-03-17 Veolia Water Solutions & Technologies Support Method and installation for treating water coming from the petroleum and gas industries, especially production water from petroleum and/or gas fields
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