CN114748885A - Production device and production process of electronic grade isopropanol - Google Patents
Production device and production process of electronic grade isopropanol Download PDFInfo
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- CN114748885A CN114748885A CN202210547768.5A CN202210547768A CN114748885A CN 114748885 A CN114748885 A CN 114748885A CN 202210547768 A CN202210547768 A CN 202210547768A CN 114748885 A CN114748885 A CN 114748885A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- 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
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- C07—ORGANIC CHEMISTRY
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- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- 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
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- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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Abstract
The invention discloses a production device and a production process of electronic grade isopropanol, and the production process comprises the following process steps: the method comprises the steps of enabling industrial grade isopropanol to enter a rectifying tower, firstly carrying out complexation reaction and dehydration treatment through a complexation processor and a dehydration processor, then entering a micro-filter to primarily filter part of impurities, then removing light components and heavy components in a multi-stage rectification mode, sending an isopropanol distillate obtained after rectification into an ion exchange processor, removing part of negative and positive ions in an ion exchange mode, sending the obtained feed liquid into a nano-filter to carry out nanofiltration treatment, and finally obtaining a water-free electronic grade isopropanol product. The method has the characteristics of strong process continuity, good separation effect, high purity, low impurity content and the like, and the process flow is easy for industrial production.
Description
Technical Field
The invention relates to the technical field of isopropanol production, in particular to a production device and a production process of electronic grade isopropanol.
Background
Electronic grade chemicals, also known as ultra-clean high-purity reagents, are one of key basic chemical materials in the process of manufacturing very large scale integrated circuits (commonly called chips), wherein electronic grade isopropanol is mainly used for ultra-clean cleaning organic solvents of cleaning, drying and cleaning workshop appliances in the process of processing precise electronic components such as chips, liquid crystals, magnetic heads, circuit boards and the like. When the ethanol contains alkali metal impurities (sodium, potassium, calcium and the like), the impurities are dissolved into the oxide film, so that the insulation voltage is reduced; when heavy metals (copper, iron, chromium, silver, etc.) are present, the P-N junction withstand voltage is lowered. Therefore, purity and cleanliness can have a significant impact on the yield, electrical performance, and reliability of integrated circuits.
However, the quality of the high-purity isopropanol product prepared by the prior art is unstable, and the processing requirement of the ultra-large scale integrated circuit is difficult to meet.
Therefore, it is an urgent need to solve the problems of the prior art to provide a production apparatus and a production process for electronic grade isopropanol with stable quality.
Disclosure of Invention
In view of this, the invention provides an electronic grade isopropanol production device and a production process thereof, and the production device has the advantages of strong process continuity, good separation effect, high purity and low impurity content.
In order to achieve the purpose, the invention adopts the following technical scheme:
an electronic grade isopropanol production device comprises a raw material storage tank, a complexing processor, a dehydration processor, a micro filter, a rectification processing system, an ion exchange processor, a nano filter and a finished product receiver which are sequentially connected through a pipeline.
By adopting the technical scheme, the invention has the beneficial effects that:
can effectively remove organic carbon, anions and cations and particle impurities in the industrial grade isopropanol raw material, and obtain the electronic grade isopropanol with higher purity.
Further, the rectification processing system comprises a plurality of rectification tower components which are connected in sequence.
Further, the number of the rectifying tower components is four, the rectifying tower components are respectively a first rectifying tower component, a second rectifying tower component, a third rectifying tower component and a fourth rectifying tower component, the first rectifying tower component, the second rectifying tower component, the third rectifying tower component and the fourth rectifying tower component have the same structure, and the first rectifying tower component, the second rectifying tower component, the third rectifying tower component and the fourth rectifying tower component all comprise an overhead condenser, a tower body and a tower kettle reboiler which are sequentially connected through pipelines from top to bottom; the microfilter is connected with the tower body of the first rectifying tower component through a pipeline; the discharge hole of the tower top condenser of the first rectifying tower component is connected with the tower body feed inlet of the second rectifying tower component through a pipeline, and similarly, the discharge hole of the tower top condenser of the second rectifying tower component is connected with the tower body feed inlet of the third rectifying tower component through a pipeline, and the discharge hole of the tower top condenser of the third rectifying tower component is connected with the tower body feed inlet of the fourth rectifying tower component through a pipeline; and the discharge hole of the condenser at the top of the tower of the fourth rectifying tower component is connected with the ion exchange processor through a pipeline.
The adoption of the further technical scheme has the beneficial effects that the purity of the distilled isopropanol can reach 99.99 percent and the impurity content reaches above SEMI international standard grade G3 through the continuous rectification operation of the four rectifying tower components.
The production process by utilizing the production device of the electronic grade isopropanol comprises the following steps:
1) firstly, industrial-grade isopropanol stored in a raw material storage tank is conveyed into a complexing processor through a raw material pump, and metal ion impurities in the industrial-grade isopropanol raw material react with a selected complexing catalyst to form impurities with larger particle sizes;
2) conveying the material obtained in the step 1) into a dewatering processor, dewatering impurities contained in isopropanol through a dewatering agent, conveying the obtained material into a micro-filter through a pump for micro-filtration, and preliminarily filtering large-particle-size solid impurities in the isopropanol raw material;
3) conveying the obtained isopropanol material to a rectification treatment system through a fluid conveying pump for rectification operation, wherein the rectification treatment system comprises four rectification tower components which are connected in sequence, namely a first rectification tower component, a second rectification tower component, a third rectification tower component and a fourth rectification tower component, in the rectification process, isopropanol is a light component, and is extracted from the top of a tower, and heavy components in a tower kettle are jointly extracted as waste liquid and recycled;
4) Conveying the isopropanol material obtained in the step 3) into an ion exchanger, further removing anion and cation impurities from the rectified product through ion exchange, and conveying the isopropanol material subjected to ion exchange operation into a nano filter for nanofiltration operation;
5) and conveying the isopropanol product subjected to nanofiltration operation to a finished product receiver for subsequent packaging.
By adopting the technical scheme, the invention has the beneficial effects that:
the process has strong continuity and good separation effect, can prepare the electronic grade isopropanol with high purity and low impurity content, and has easy industrial production.
Further, the dehydrating agent in step 2) is any one of molecular sieve, magnesium sulfate, calcium chloride, acid anhydride and silica gel.
Further, the medium applied to the nanofiltration membrane of the nanofiltration membrane in the step 4) is high-purity isopropanol.
The method has the advantages that the problem that separation performance is reduced due to the fact that the nanofiltration membrane used for water treatment is easy to swell in an organic solvent is avoided, and the nanofiltration membrane is made of an organic solvent nanofiltration membrane material and can be stably used in high-purity isopropanol for a long time.
Further, in the step 1), the complexing catalyst is an organic silicon high-molecular metal complexing agent.
The organic silicon polymer metal complexing agent is prepared by addition of diallyl crown ether and hydrogen-containing silicone oil, has the advantages of easiness in processing, low price, low toxicity and convenience in recovery, has a certain cavity in a crown ether molecule, can be used for drilling metal ions into the cavity to be complexed with ether bonds, has a large complexing constant and high selectivity, and can greatly reduce the content of heavy metal ions in a product.
Furthermore, in the step 2), the micro-filtration membrane of the micro-filter is made of high-density polyethylene, the caliber is 0.2-0.8 μm, and the filtration pressure during filtration is 0.5-0.8 MPa.
Further, in the step 3), the absolute pressure of the top of the first rectifying tower component is 0.1-0.3 Mpa, the reflux ratio is 2-8, the temperature of the tower kettle is set to be 70-120 ℃, and the reflux temperature is 60-110 ℃; the absolute pressure at the top of the second rectifying tower component is 0.1-0.3 Mpa, the reflux ratio is 4-10, the temperature of the tower kettle is set to be 60-120 ℃, and the reflux temperature is 60-114 ℃; the absolute pressure at the top of the third rectifying tower component is 0.1-0.3 Mpa, the reflux ratio is 5-12, the temperature of the tower kettle is set to be 70-115 ℃, and the reflux temperature is 55-98 ℃; the absolute pressure at the top of the fourth rectifying tower component is 0.1-0.3 Mpa, the reflux ratio is 6-15, the temperature of the tower kettle is 70-130 ℃, and the reflux temperature at the top of the tower is 65-95 ℃.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic structural diagram of an electronic grade isopropanol production device provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1:
as shown in fig. 1, the embodiment of the invention discloses an electronic grade isopropanol production device, which comprises a raw material storage tank 1, a complexing processor 2, a dewatering processor 3, a microfilter 4, a first rectifying tower component 5, a second rectifying tower component 6, a third rectifying tower component 7, a fourth rectifying tower component 8, an ion exchange processor 9, a nanofiltration device 10 and a finished product receiver 11 which are sequentially connected through pipelines;
The first rectifying tower component 5, the second rectifying tower component 6, the third rectifying tower component 7 and the fourth rectifying tower component 8 are identical in structure and respectively comprise an overhead condenser 12, a tower body and a tower kettle reboiler 13 which are connected in sequence from top to bottom through pipelines; the microfilter 4 is connected with the tower body of the first rectifying tower component 5 through a pipeline; a discharge hole of the tower top condenser 12 of the first rectifying tower component 5 is connected with a tower body feed inlet of the second rectifying tower component 6 through a pipeline, similarly, a discharge hole of the tower top condenser 12 of the second rectifying tower component 6 is connected with a tower body feed inlet of the third rectifying tower component 7 through a pipeline, and a discharge hole of the tower top condenser 12 of the third rectifying tower component 7 is connected with a tower body feed inlet of the fourth rectifying tower component 8 through a pipeline; the discharge port of the tower top condenser 12 of the fourth rectifying tower component 8 is connected with the ion exchange processor through a pipeline.
The method can effectively remove organic carbon, anions and cations and particle impurities in the industrial grade isopropanol raw material, and obtain the electronic grade isopropanol with higher purity.
The embodiment of the invention also discloses a production process by utilizing the production device, which comprises the following steps:
1) firstly, industrial-grade isopropanol stored in a raw material storage tank 1 is conveyed into a complexing processor 2 through a raw material pump, so that metal ion impurities in the industrial-grade isopropanol raw material react with a selected complexing catalyst to form impurities with larger particle size, and subsequent further treatment is facilitated;
In the step, the complexing catalyst is a metal complexing agent, the mass in the process is preferably 0.2-2.0% of the total mass of the industrial grade isopropanol raw material, the metal complexing agent is an organic silicon high-molecular complexing agent prepared by adding diallyl crown ether and hydrogen-containing silicone oil, the high-molecular metal ion complexing agent in the process can be effectively recovered and recycled through chemical treatment, in the step, the operating condition in the complexing processor 2 is normal temperature and normal pressure, and the retention time of reactants is 30-60 min;
in the embodiment, the industrial isopropanol with the purity of more than or equal to 99.9 percent is stored in the raw material storage tank 1; the mass of the metal complexing agent is selected to be 0.3 percent of the total mass of the industrial grade isopropanol raw material, and the retention time of reactants is 50 min.
2) Conveying the material obtained in the step 1) into a dewatering processor 3, dewatering impurities contained in isopropanol by using a dewatering agent, conveying the obtained material into a micro-filter 4 by using a pump for micro-filtration, and preliminarily filtering large-particle-size solid impurities in the isopropanol raw material to prepare for further removing other impurities in the isopropanol;
it should be noted that the dehydrating agent in this step may be any one of molecular sieve, magnesium sulfate, calcium chloride, acid anhydride and silica gel, the mass of the dehydrating agent is preferably 0.1-1.0% of the mass of the isopropanol material, and the operating conditions of the dehydrating processor 3 are normal pressure, 60-100 ℃, and the reaction time is 60-120 min.
In this example, the dehydrating agent is calcium chloride, the mass of the dehydrating agent is 0.1% of the mass of the isopropyl alcohol material, and the operating conditions of the dehydrating processor 3 are as follows: the reaction time is 60min at the normal pressure and 60 ℃.
In the step 2), the microfiltration membrane of the microfilter 4 is made of high density polyethylene, the caliber is 0.2-0.8 μm, and the filtering pressure during filtering is 0.5-0.8 MPa.
In this example, the microfiltration membrane is made of high density polyethylene, and has a diameter of 0.2 μm, and the filtration pressure during microfiltration is selected to be 0.5 MPa.
3) Conveying the obtained isopropanol material to a rectification treatment system through a fluid conveying pump for rectification operation, wherein the rectification treatment system comprises four rectification tower components which are connected in sequence, namely a first rectification tower component 5, a second rectification tower component 6, a third rectification tower component 7 and a fourth rectification tower component 8, in the rectification process, isopropanol is a light component and is extracted from the top of the tower, and heavy components in a tower kettle are jointly extracted as waste liquid and recycled;
the step needs to be explained, the absolute pressure at the top of the first rectifying tower component 5 is 0.1-0.3 Mpa, the reflux ratio is 2-8, the temperature of the tower kettle is set to be 70-120 ℃, and the reflux temperature is 60-110 ℃; the absolute pressure at the top of the second rectifying tower component 6 is 0.1-0.3 Mpa, the reflux ratio is 4-10, the temperature of a tower kettle is set to be 60-120 ℃, and the reflux temperature is 60-114 ℃; the absolute pressure at the top of the third rectifying tower component 7 is 0.1-0.3 Mpa, the reflux ratio is 5-12, the temperature of a tower kettle is set to be 70-115 ℃, and the reflux temperature is 55-98 ℃; the absolute pressure at the top of the fourth rectifying tower component 8 is 0.1-0.3 Mpa, the reflux ratio is 6-15, the temperature of the tower kettle is set to be 70-130 ℃, and the reflux temperature at the top of the tower is 65-95 ℃.
In the embodiment, the reflux ratio of the first rectifying tower component 5 is 2, the temperature of the tower kettle is set to be 80 ℃, and the reflux temperature at the top of the tower is 70 ℃; the reflux ratio of the second rectifying tower assembly 6 is 3, the temperature of a tower kettle is set to be 70 ℃, and the reflux temperature of the tower top is 70 ℃; the reflux ratio of the third rectifying tower component 7 is 5, the temperature of a tower kettle is set to be 80 ℃, and the reflux temperature of the tower top is 70 ℃; the reflux ratio of the fourth rectifying tower component 8 is 5, the temperature of the tower bottom is set to be 80 ℃, and the reflux temperature of the tower top is 70 ℃.
4) Conveying the isopropanol material obtained in the step 3) into an ion exchanger 9, further removing anion and cation impurities from the rectified product through ion exchange, and conveying the isopropanol material subjected to the ion exchange operation into a nano filter 10 for nanofiltration operation;
it should be noted that the nanofiltration membrane of the nanofiltration membrane 10 uses high-purity isopropanol as a medium, and the traditional nanofiltration membrane used for water treatment is likely to swell in an organic solvent to cause the reduction of separation performance, so that the nanofiltration membrane is difficult to be competent.
5) The isopropanol product after nanofiltration is transferred to a finished product receiver 11 to become electronic grade isopropanol.
The method has the advantages of strong process continuity and good separation effect, can prepare the electronic grade isopropanol with high purity and low impurity content, and has easy process flow for industrial production.
The electronic grade isopropanol impurity index of the embodiment is detected as follows:
| categories | Index (I) |
| Content of isopropyl alcohol/%) | 99.99 |
| Particles (not less than 0.2 μm and not more than 0.5 μm) are in each |
6 |
| Total Organic Carbon (TOC). times.10-6 | 6 |
| Chloride (Cl). times.10-9 | 11 |
| Sulfate (SO)4）×10-9 | 35 |
| Nitrate (PO)4）×10-9 | 39 |
| Phosphate (PO)4）×10-9 | 21 |
| Aluminum (Al). times.10-9 | 0.08 |
| Arsenic (As). times.10-9 | 0.06 |
| Barium (Ba). times.10-9 | 0.09 |
| Calcium (Ca). times.10-9 | 0.11 |
Example 2:
as shown in fig. 1, the embodiment of the invention discloses an electronic grade isopropanol production device, which comprises a raw material storage tank 1, a complexing processor 2, a dewatering processor 3, a microfilter 4, a first rectifying tower component 5, a second rectifying tower component 6, a third rectifying tower component 7, a fourth rectifying tower component 8, an ion exchange processor 9, a nanofiltration device 10 and a finished product receiver 11 which are sequentially connected through a pipeline;
the first rectifying tower component 5, the second rectifying tower component 6, the third rectifying tower component 7 and the fourth rectifying tower component 8 are identical in structure and respectively comprise an overhead condenser 12, a tower body and a tower kettle reboiler 13 which are connected in sequence from top to bottom through pipelines; the microfilter 4 is connected with the tower body of the first rectifying tower component 5 through a pipeline; a discharge hole of the tower top condenser 12 of the first rectifying tower component 5 is connected with a tower body feed inlet of the second rectifying tower component 6 through a pipeline, similarly, a discharge hole of the tower top condenser 12 of the second rectifying tower component 6 is connected with a tower body feed inlet of the third rectifying tower component 7 through a pipeline, and a discharge hole of the tower top condenser 12 of the third rectifying tower component 7 is connected with a tower body feed inlet of the fourth rectifying tower component 8 through a pipeline; the discharge port of the tower top condenser 12 of the fourth rectifying tower component 8 is connected with the ion exchange processor through a pipeline.
The method can effectively remove organic carbon, anions and particle impurities in the industrial grade isopropanol raw material, and obtain the electronic grade isopropanol with higher purity.
The embodiment of the invention also discloses a production process by utilizing the production device, which comprises the following steps:
1) firstly, industrial-grade isopropanol stored in a raw material storage tank 1 is conveyed into a complexing processor 2 through a raw material pump, so that metal ion impurities in the industrial-grade isopropanol raw material react with a selected complexing catalyst to form impurities with larger particle size, and subsequent further treatment is facilitated;
it should be noted that the complexing catalyst in this step is a metal complexing agent, the mass in the process should be selected to be 0.2% -2.0% of the total mass of the industrial grade isopropanol raw material, the metal complexing agent is an organosilicon polymer complexing agent prepared by the addition of diallyl crown ether and hydrogen-containing silicone oil, and the polymer metal ion complexing agent in the process can be effectively recovered and recycled through chemical treatment. In the step, the operating conditions in the complexing processor 2 are normal temperature and normal pressure, and the residence time of reactants is 30-60 min;
in the embodiment, the industrial isopropanol with the purity of more than or equal to 98 percent is stored in a raw material storage tank 1; the mass of the metal complexing agent is selected to be 0.5 percent of the total mass of the industrial grade isopropanol raw material, and the retention time of reactants is 85 min.
2) Conveying the material obtained in the step 1) into a dewatering processor 3, dewatering impurities contained in isopropanol by using a dewatering agent, conveying the obtained material into a micro-filter 4 by using a pump for micro-filtration, and preliminarily filtering large-particle-size solid impurities in the isopropanol raw material to prepare for further removing other impurities in the isopropanol;
it should be noted that the dehydrating agent in this step may be any one of molecular sieve, magnesium sulfate, calcium chloride, acid anhydride and silica gel, the mass of the dehydrating agent is preferably 0.1-1.0% of the mass of the isopropyl alcohol material, and the operating conditions of the dehydrating processor 3 are normal pressure, 60-100 ℃, and the reaction time is 60-120 min.
In this example, the dehydrating agent is a molecular sieve, the mass of the dehydrating agent is 1.3% of the mass of the isopropyl alcohol material, and the operating conditions of the dehydrating processor 3 are as follows: the reaction time is 120min at the normal pressure and 100 ℃.
In the step 2), the microfiltration membrane of the microfiltration device 4 is made of high density polyethylene, the aperture is 0.2-0.8 μm, and the filtration pressure during filtration is 0.5-0.8 MPa.
In this embodiment, the microfiltration membrane is made of high density polyethylene, and has a diameter of 0.8 μm, and the filtration pressure during microfiltration is selected to be 0.8 MPa.
3) Conveying the obtained isopropanol material to a rectification treatment system through a fluid conveying pump for rectification operation, wherein the rectification treatment system comprises four rectification tower components which are connected in sequence, namely a first rectification tower component 5, a second rectification tower component 6, a third rectification tower component 7 and a fourth rectification tower component 8, in the rectification process, isopropanol is a light component and is extracted from the top of the tower, and heavy components in a tower kettle are jointly extracted as waste liquid and recycled;
the step needs to be described, wherein the absolute pressure at the top of the first rectifying tower component 5 is 0.1-0.3 Mpa, the reflux ratio is 2-8, the temperature of a tower kettle is set to be 70-120 ℃, and the reflux temperature is 60-110 ℃; the absolute pressure at the top of the second rectifying tower component 6 is 0.1-0.3 Mpa, the reflux ratio is 4-10, the temperature of a tower kettle is set to be 60-120 ℃, and the reflux temperature is 60-114 ℃; the absolute pressure at the top of the third rectifying tower component 7 is 0.1-0.3 Mpa, the reflux ratio is 5-12, the temperature of a tower kettle is set to be 70-115 ℃, and the reflux temperature is 55-98 ℃; the absolute pressure at the top of the fourth rectifying tower component 8 is 0.1-0.3 Mpa, the reflux ratio is 6-15, the temperature of the tower kettle is set to be 70-130 ℃, and the reflux temperature at the top of the tower is 65-95 ℃.
In the embodiment, the reflux ratio of the first rectifying tower component 5 is 5, the temperature of the tower kettle is set to be 110 ℃, and the reflux temperature of the tower top is 80 ℃; the reflux ratio of the second rectifying tower component 6 is 8, the temperature of a tower kettle is set to be 100 ℃, and the reflux temperature of the tower top is 80 ℃; the reflux ratio of the third rectifying tower component 7 is 10, the temperature of a tower kettle is set to be 110 ℃, and the reflux temperature of the tower top is 80 ℃; the reflux ratio of the fourth rectifying tower component 8 is 10, the temperature of the tower bottom is set to be 120 ℃, and the reflux temperature of the tower top is 80 ℃.
4) Conveying the isopropanol material obtained in the step 3) into an ion exchanger 9, further removing anion and cation impurities from the rectified product through ion exchange, and conveying the isopropanol material subjected to ion exchange operation into a nano filter 10 for nanofiltration operation;
it should be noted that the nanofiltration membrane of the nanofiltration membrane 10 uses high-purity isopropanol as a medium, and the traditional nanofiltration membrane used for water treatment is likely to swell in an organic solvent to cause the reduction of separation performance, so that the nanofiltration membrane is difficult to be competent.
5) The isopropyl alcohol product after nanofiltration is transferred to a finished product receiver 11 to become electronic grade isopropyl alcohol.
The method has the advantages of strong process continuity and good separation effect, can prepare the electronic grade isopropanol with high purity and low impurity content, and has easy process flow for industrial production.
The electronic grade isopropanol impurity index of the embodiment is detected as follows:
| categories | Index (es) |
| Content of isopropyl alcohol/%) | 99.99 |
| Particles (not less than 0.2 mu m and not more than 0.5 mu m) are mL-1 | 8 |
| Total Organic Carbon (TOC). times.10-6 | 6 |
| Chloride (Cl). times.10-9 | 13 |
| Sulfate (SO 4) x 10-9 | 32 |
| Nitrate (PO 4). times.10-9 | 41 |
| Phosphate (PO 4). times.10-9 | 26 |
| Aluminum (Al) x 10-9 | 0.09 |
| Arsenic (As). times.10-9 | 0.05 |
| Barium (Ba). times.10-9 | 0.09 |
| Calcium (Ca). times.10-9 | 0.11 |
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. An electronic grade isopropanol production device is characterized by comprising a raw material storage tank, a complexing processor, a dewatering processor, a micro filter, a rectification processing system, an ion exchange processor, a nano filter and a finished product receiver which are sequentially connected through a pipeline.
2. The apparatus of claim 1 wherein the rectification processing system comprises a plurality of rectification column assemblies connected in series.
3. The production device of the electronic grade isopropanol according to claim 2, wherein the number of the rectifying tower components is four, the four rectifying tower components are respectively a first rectifying tower component, a second rectifying tower component, a third rectifying tower component and a fourth rectifying tower component, the first rectifying tower component, the second rectifying tower component, the third rectifying tower component and the fourth rectifying tower component have the same structure, and each rectifying tower component comprises an overhead condenser, a tower body and a kettle reboiler which are sequentially connected through pipelines from top to bottom; the microfilter is connected with the tower body of the first rectifying tower component through a pipeline; the discharge hole of the overhead condenser of the first rectifying tower component is connected with the tower body feed inlet of the second rectifying tower component through a pipeline, and similarly, the discharge hole of the overhead condenser of the second rectifying tower component is connected with the tower body feed inlet of the third rectifying tower component through a pipeline, and the discharge hole of the overhead condenser of the third rectifying tower component is connected with the tower body feed inlet of the fourth rectifying tower component through a pipeline; and the discharge hole of the tower top condenser of the fourth rectifying tower component is connected with the ion exchange processor through a pipeline.
4. A process according to any one of claims 1 to 3, comprising the following steps:
1) firstly, industrial-grade isopropanol stored in a raw material storage tank is conveyed into a complexing processor through a raw material pump, and metal ion impurities in the industrial-grade isopropanol raw material react with a selected complexing catalyst to form impurities with larger particle sizes;
2) conveying the material obtained in the step 1) to a dewatering processor, dewatering impurities contained in isopropanol by using a dewatering agent, conveying the obtained material to a micro-filter by using a pump for micro-filtration, and primarily filtering large-particle-size solid impurities in the isopropanol raw material;
3) conveying the obtained isopropanol material to a rectification treatment system through a fluid conveying pump for rectification operation, wherein the rectification treatment system comprises four rectification tower components which are connected in sequence, namely a first rectification tower component, a second rectification tower component, a third rectification tower component and a fourth rectification tower component, in the rectification process, isopropanol is a light component and is extracted from the top of the tower, and heavy components in the tower bottom are jointly extracted as waste liquid and recycled;
4) Conveying the isopropanol material obtained in the step 3) into an ion exchanger, further removing anion and cation impurities from the rectified product through ion exchange, and conveying the isopropanol material subjected to ion exchange operation into a nano filter for nanofiltration operation;
5) and conveying the isopropanol product subjected to nanofiltration operation to a finished product receiver for subsequent packaging.
5. The process for producing electronic grade isopropanol according to claim 4, wherein the dehydrating agent in step 2) is any one of molecular sieve, magnesium sulfate, calcium chloride, acid anhydride and silica gel.
6. The process for producing electronic grade isopropanol according to claim 4, wherein the nanofiltration membrane of the nanofiltration membrane in step 4) uses high purity isopropanol.
7. The process according to claim 4, wherein the complexing catalyst in step 1) is an organosilicon polymer metal complexing agent.
8. The process for producing electronic grade isopropanol as claimed in claim 4, wherein the microfiltration membrane of the microfilter in step 2) is made of high density polyethylene, and has a pore size of 0.2-0.8 μm and a filtration pressure of 0.5-0.8 MPa.
9. The process for producing electronic grade isopropanol according to claim 4, wherein in step 3), the top absolute pressure of the first rectifying tower component is 0.1-0.3 Mpa, the reflux ratio is 2-8, the temperature of the tower kettle is set to be 70-120 ℃, and the reflux temperature is 60-110 ℃; the absolute pressure at the top of the second rectifying tower component is 0.1-0.3 Mpa, the reflux ratio is 4-10, the temperature of the tower kettle is set to be 60-120 ℃, and the reflux temperature is 60-114 ℃; the absolute pressure at the top of the third rectifying tower component is 0.1-0.3 Mpa, the reflux ratio is 5-12, the temperature of the tower kettle is set to be 70-115 ℃, and the reflux temperature is 55-98 ℃; the absolute pressure at the top of the fourth rectifying tower component is 0.1-0.3 Mpa, the reflux ratio is 6-15, the temperature of the tower kettle is set to be 70-130 ℃, and the reflux temperature at the top of the tower is 65-95 ℃.
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