CN112409135A - Preparation method of high-purity isopropanol - Google Patents
Preparation method of high-purity isopropanol Download PDFInfo
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- CN112409135A CN112409135A CN202011223776.1A CN202011223776A CN112409135A CN 112409135 A CN112409135 A CN 112409135A CN 202011223776 A CN202011223776 A CN 202011223776A CN 112409135 A CN112409135 A CN 112409135A
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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
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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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
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Abstract
The invention discloses a preparation method of high-purity isopropanol, which comprises the following steps: (1) crude isopropanol: acetone and hydrogen are used as raw materials, isopropanol is used as a solvent, the raw materials are contacted with a catalyst, and the reaction is carried out to generate the isopropanol, wherein the catalyst comprises the following components: a) a silica support, b) nickel or an oxide thereof, c) at least one of MgO, BaO or CaO; (2) resin dehydration: flowing the prepared isopropyl alcohol through a water absorbent resin at a constant flow rate; (3) reverse osmosis: passing the isopropanol after resin dehydration through a reverse osmosis membrane; (4) high-temperature rectification: rectifying the isopropanol subjected to reverse osmosis at high temperature; (5) and canning the rectified high-purity isopropanol. The invention takes acetone and hydrogen as raw materials to prepare isopropanol, and then comprehensively uses a plurality of means to purify the isopropanol, the design of the purification route is reasonable and ingenious, and the finally obtained acetone conversion rate can reach more than 96 percent.
Description
Technical Field
The invention relates to a method for preparing isopropanol, in particular to a method for preparing high-purity isopropanol.
Background
The production of isopropanol may be achieved by hydration of propylene, such as by direct hydration with a cation exchange resin catalyst.
In recent years, the yield of acetone has been increasing, but since the production process of methyl methacrylate tends to replace the acetone cyanohydrin process by the direct oxidation process of the C4 fraction and the use of acetone as a solvent is decreasing, narrowing the application range of acetone, it is of great importance to convert acetone into isopropanol fine chemicals. The catalysts for the acetone hydrogenation crude isopropanol so far include: raney Ni catalyst, Ru/C catalyst, Ru/Al2O3 catalyst and Cu-Cr catalyst. Acetone is hydrogenated on the above type of catalyst, generally a fixed bed reactor is adopted, acetone and hydrogen enter a catalyst bed layer in a certain proportion under the condition of liquid phase or gas phase, and isopropanol is generated by hydrogenation under proper temperature and pressure.
Chinese patent CN103539635B reports a method for preparing isopropanol by gas phase reaction of acetone as raw material and hydrogen gas through acid-treated silica carrier loaded with nickel element and its compound. By adopting the method, high-purity isopropanol for the pharmaceutical and cosmetic industries can be obtained through subsequent processing. However, the nickel and cobalt content in the supported nickel catalyst in the method is higher, so that the preparation cost of the catalyst is higher, and the economy of preparing isopropanol by hydrogenating acetone is reduced.
Disclosure of Invention
The invention aims to solve the technical problems that a Pd, Pt and Ru noble metal catalyst prepared by the prior art is expensive when used in the process of preparing isopropanol by acetone hydrogenation, and a Cu-based catalyst has the problems of poor stability, serious environmental pollution and the like when used in the process of preparing isopropanol by acetone hydrogenation, and provides a novel method for preparing isopropanol by acetone gas-phase hydrogenation. The method has the advantages of low catalyst price, good stability and environmental friendliness.
To solve the above-mentioned technology, the technical scheme adopted by the invention is as follows: a preparation method of high-purity isopropanol comprises the following steps:
(1) crude isopropanol: the method comprises the following steps of taking acetone and hydrogen as raw materials, taking isopropanol as a solvent, wherein the mixture of the raw materials and the solvent comprises, by weight, 10-80% of acetone and 20-90% of isopropanol, and the raw materials and the catalyst are contacted at a reaction temperature of 100-160 ℃ and a reaction pressure of 1.0-5.0 MPa to react to generate the isopropanol, wherein the catalyst comprises the following components in percentage by weight: a) 40-97.5 parts of silicon dioxide carrier which is treated by acid, and b) 0.5-60 parts of nickel element or oxide thereof loaded on the silicon dioxide carrier, c) 3.0-15.0% of at least one of MgO, BaO or CaO;
(2) resin dehydration: enabling the prepared isopropanol to flow through the water-absorbing resin at a constant flow rate, and controlling the water content of the isopropanol to be reduced to below 20 ppm;
(3) reverse osmosis: enabling isopropanol after resin dehydration to pass through a reverse osmosis membrane, wherein the reverse osmosis pressure is 2.0-2.8Mpa, the permeability is 400-900L/h, and the circulation amount is controlled to be 700-900L/h;
(4) high-temperature rectification: rectifying the isopropanol subjected to reverse osmosis at high temperature, controlling the temperature of the top of the tower to be 82.0 +/-0.5 ℃, the reflux ratio to be 1.2-2, the temperature of condensed water to be less than 4-8 ℃, controlling the concentration of anions in the isopropanol after rectification at high temperature to be below 100ppb, and controlling the concentration of single cations to be below 1 ppb;
(5) and canning the rectified high-purity isopropanol.
Furthermore, the mixture of the raw materials and the solvent contains 25.0-70.0% of acetone and 30.0-65.0% of isopropanol by weight percentage.
Furthermore, the amount of at least one of MgO, BaO and CaO is 5.0-10.0% by weight.
Further, in the step (2), the water-absorbent resin is polyacrylic acid water-absorbent resin.
Further, the preparation method of the catalyst comprises the following steps: adding nickel nitrate into a hydrochloric acid solution, carrying out ultrasonic stirring in an ultrasonic instrument to completely dissolve the nickel nitrate, then adding carrier silicon dioxide, adding at least one of MgO, BaO or CaO into the solution which is pasty fluid, and placing the solution in an ultrasonic cleaning instrument for ultrasonic stirring to fully dissolve the solution; then drying and roasting to obtain the catalyst; wherein: the molar ratio of the carrier silicon dioxide, the nickel nitrate and the hydrochloric acid solution is 1-1.02: 0.3-0.5: 1.05; the concentration of the hydrochloric acid solution is 15-30%.
Furthermore, the time of ultrasonic stirring in an ultrasonic instrument is 13-17 minutes, the time of ultrasonic placing in an ultrasonic cleaning instrument is 13-17 minutes, the roasting temperature is 450-550 ℃, and the roasting time is 4-5 hours.
Compared with the method for preparing isopropanol by catalytically hydrogenating acetone by using noble metal, the catalyst provided by the method is low in price, and in the process of generating isopropanol by hydrogenating acetone, part of acetone can be directly coupled to generate methyl isobutyl ketone, and the generated isopropanol is also easily etherified to form a byproduct. Therefore, the acid sites of the catalyst need to be matched with the hydrogenation activity, and the acid center number and the acid strength of the catalyst are adjusted by introducing basic oxides into the carrier; the hydrogenation activity of the catalyst needs to be controlled by reasonably controlling the content of Ni, so that the prepared Ni-based metal catalyst maintains good activity, stability and selectivity. Compared with a noble metal Ru catalyst, the catalyst is low in price, the reaction is carried out under 1.0-5.0 MPa, and the pressure is low. The catalyst has high activity compared to Cu-based catalysts.
By adopting the method, the catalyst is prepared by a chemical reduction method, isopropanol is used as a solvent, the reaction condition of the reaction temperature of 100-160 ℃ and the reaction pressure of 1.0-5.0 MPa is applied to the process of synthesizing isopropanol by acetone hydrogenation, the conversion rate of acetone can reach more than 96% after the reaction is carried out for 4 hours, and the selectivity of the generated isopropanol is more than 95%. And then, the isopropanol is purified by comprehensively using a plurality of means, the design of the purification route is reasonably and skillfully designed, and finally the high-purity isopropanol with each single cation concentration of less than 10ppt, each single anion concentration of less than 1ppb and the moisture content of less than 20ppm can be obtained. Compared with a noble metal catalyst, the catalyst has low price and low reaction pressure, and compared with a Cu-based catalyst, the catalyst has high activity and obtains good technical effect.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, but the scope of the present invention is not limited thereto.
Example 1
A preparation method of high-purity isopropanol comprises the following steps:
(1) crude isopropanol: acetone and hydrogen are used as raw materials, isopropanol is used as a solvent, the mixture of the raw materials and the solvent comprises, by weight, 30-70% of acetone and 30-65% of isopropanol, the raw materials and a catalyst are contacted at a reaction temperature of 160 ℃ and a reaction pressure of 3.0MPa to react to generate the isopropanol, wherein the catalyst comprises the following components in percentage by weight: a)40 parts of silica carrier which is treated by acid, and b) 0.5-60 parts of nickel element or oxide thereof loaded on the silica carrier, c) 5% of MgO;
(2) resin dehydration: enabling the prepared isopropanol to flow through polyacrylic acid water-absorbing resin at a constant flow rate, and controlling the water content of the isopropanol to be reduced to below 20 ppm;
(3) reverse osmosis: allowing the isopropanol after resin dehydration to pass through a reverse osmosis membrane, wherein the reverse osmosis pressure is 2.0Mpa, the permeation amount is 400L/h, and the circulation amount is controlled to be 700L/h;
(4) high-temperature rectification: rectifying the isopropanol subjected to reverse osmosis at high temperature, controlling the temperature of the top of the tower to be 81.5 ℃, the reflux ratio to be 1.2-2, controlling the temperature of condensed water to be less than 8 ℃, controlling the concentration of anions in the isopropanol subjected to high-temperature rectification to be less than 100ppb, and controlling the concentration of single cations to be less than 1 ppb;
(5) the yield of the rectified isopropanol product is 97.5 percent, the purity is 99.6 percent, and the rectified high-purity isopropanol is canned.
In this example, the preparation method of the catalyst: adding nickel nitrate into a hydrochloric acid solution, carrying out ultrasonic stirring in an ultrasonic instrument to completely dissolve the nickel nitrate, then adding carrier silicon dioxide, adding MgO, and placing the mixture into an ultrasonic cleaning instrument to carry out ultrasonic stirring to fully dissolve the solution, wherein the solution is a sticky fluid; then drying and roasting to obtain the catalyst; wherein: the molar ratio of the carrier silicon dioxide, the nickel nitrate and the hydrochloric acid solution is 1-1.02: 0.3-0.5: 1.05; the concentration of the hydrochloric acid solution is 15-30%. The time of ultrasonic stirring in an ultrasonic instrument is 15 minutes, the time of ultrasonic cleaning in an ultrasonic cleaning instrument is 15 minutes, the roasting temperature is 450 ℃, and the roasting time is 4-5 hours.
Example 2
The catalyst preparation method is the same as that of example 1, (3) reverse osmosis: allowing the isopropanol after resin dehydration to pass through a reverse osmosis membrane, wherein the reverse osmosis pressure is 2.5Mpa, the permeation amount is 500L/h, and the circulation amount is controlled to be 800L/h; (4) high-temperature rectification: rectifying the isopropanol after reverse osmosis at high temperature, controlling the temperature of the top of the tower to be 81.5 ℃, the reflux ratio to be 1.2-2 and the temperature of condensed water to be less than 8 ℃. In this example, the yield of the isopropyl alcohol product was 97.4% and the purity was 99.4%.
Example 3
The catalyst preparation method is the same as that of example 1, (3) reverse osmosis: allowing the isopropanol after resin dehydration to pass through a reverse osmosis membrane, wherein the reverse osmosis pressure is 2.8Mpa, the permeation amount is 600L/h, and the circulation amount is controlled to be 900L/h; (4) high-temperature rectification: rectifying the isopropanol after reverse osmosis at high temperature, controlling the temperature of the top of the tower to be 81.5 ℃, the reflux ratio to be 1.2-2 and the temperature of condensed water to be less than 8 ℃. In this example, the yield of the rectified isopropanol product was 97.5%, and the purity was 99.6%.
Example 4
A preparation method of high-purity isopropanol comprises the following steps:
(1) crude isopropanol: acetone and hydrogen are used as raw materials, isopropanol is used as a solvent, the mixture of the raw materials and the solvent comprises, by weight, 30-70% of acetone and 30-65% of isopropanol, the raw materials and a catalyst are contacted at a reaction temperature of 130 ℃ and a reaction pressure of 3.0MPa to react to generate the isopropanol, wherein the catalyst comprises the following components in percentage by weight: a)60 parts of an acid-treated silica carrier, and supported thereon b)30 parts of nickel element or an oxide thereof, c) 5.0% of BaO;
(2) resin dehydration: enabling the prepared isopropanol to flow through polyacrylic acid water-absorbing resin at a constant flow rate, and controlling the water content of the isopropanol to be reduced to below 20 ppm;
(3) reverse osmosis: allowing the isopropanol after resin dehydration to pass through a reverse osmosis membrane, wherein the reverse osmosis pressure is 2.0Mpa, the permeation amount is 400L/h, and the circulation amount is controlled to be 700L/h;
(4) high-temperature rectification: rectifying the isopropanol subjected to reverse osmosis at high temperature, controlling the temperature of the top of the tower to be 82.0 ℃, the reflux ratio to be 1.2-2, the temperature of condensed water to be less than 8 ℃, controlling the concentration of anions in the isopropanol subjected to high-temperature rectification to be less than 100ppb, and controlling the concentration of single cations to be less than 1 ppb;
(5) the yield of the rectified isopropanol product is 96.8 percent, the purity is 99.4 percent, and the rectified high-purity isopropanol is canned.
Further, the preparation method of the catalyst comprises the following steps: adding nickel nitrate into a hydrochloric acid solution, carrying out ultrasonic stirring in an ultrasonic instrument to completely dissolve the nickel nitrate, then adding carrier silicon dioxide, adding BaO, and placing the mixture into an ultrasonic cleaning instrument to carry out ultrasonic stirring to fully dissolve the solution, wherein the solution is a sticky fluid; then drying and roasting to obtain the catalyst; wherein: the molar ratio of the carrier silicon dioxide, the nickel nitrate and the hydrochloric acid solution is 1-1.02: 0.3-0.5: 1.05; the concentration of the hydrochloric acid solution is 15-30%, the ultrasonic stirring time in an ultrasonic wave instrument is 15 minutes, the ultrasonic time in an ultrasonic cleaning instrument is 15 minutes, the roasting temperature is 500 ℃, and the roasting time is 4-5 hours.
Example 5
The catalyst preparation method is the same as that of example 4, (3) reverse osmosis: allowing the isopropanol after resin dehydration to pass through a reverse osmosis membrane, wherein the reverse osmosis pressure is 2.5Mpa, the permeation amount is 500L/h, and the circulation amount is controlled to be 800L/h; (4) high-temperature rectification: rectifying the isopropanol after reverse osmosis at high temperature, controlling the tower top temperature to be 82 ℃, the reflux ratio to be 1.2-2 and the temperature of condensed water to be less than 8 ℃. In this example, the yield of the isopropyl alcohol product was 97.2% and the purity was 99.4%.
Example 6
The catalyst preparation method is the same as that of example 4, (3) reverse osmosis: allowing the isopropanol after resin dehydration to pass through a reverse osmosis membrane, wherein the reverse osmosis pressure is 2.8Mpa, the permeation amount is 600L/h, and the circulation amount is controlled to be 900L/h; (4) high-temperature rectification: rectifying the isopropanol after reverse osmosis at high temperature, controlling the tower top temperature to be 82 ℃, the reflux ratio to be 1.2-2 and the temperature of condensed water to be less than 8 ℃. In this example, the yield of the rectified isopropanol product was 97.3%, and the purity was 99.2%.
Example 7
A preparation method of high-purity isopropanol comprises the following steps:
(1) crude isopropanol: acetone and hydrogen are used as raw materials, isopropanol is used as a solvent, the mixture of the raw materials and the solvent comprises, by weight, 30-70% of acetone and 30-65% of isopropanol, the raw materials and a catalyst are contacted at a reaction temperature of 100 ℃ and a reaction pressure of 3.0MPa to react to generate the isopropanol, wherein the catalyst comprises the following components in percentage by weight: a) 40-97.5 parts of silicon dioxide carrier subjected to acid treatment, and b) 0.5-60 parts of nickel element or oxide thereof loaded on the silicon dioxide carrier, c) 5.0% of CaO;
(2) resin dehydration: enabling the prepared isopropanol to flow through polyacrylic acid water-absorbing resin at a constant flow rate, and controlling the water content of the isopropanol to be reduced to below 20 ppm;
(3) reverse osmosis: enabling isopropanol after resin dehydration to pass through a reverse osmosis membrane, wherein the reverse osmosis pressure is 2.0-2.8Mpa, the permeability is 400-900L/h, and the circulation amount is controlled to be 700-900L/h;
(4) high-temperature rectification: rectifying the isopropanol subjected to reverse osmosis at high temperature, controlling the temperature of the top of the tower to be 82.0 +/-0.5 ℃, the reflux ratio to be 1.2-2, the temperature of condensed water to be less than 4-8 ℃, controlling the concentration of anions in the isopropanol after rectification at high temperature to be below 100ppb, and controlling the concentration of single cations to be below 1 ppb;
(5) the yield of the rectified isopropanol product is 97.5 percent, the purity is 99.6 percent, and the rectified high-purity isopropanol is canned.
Further, the preparation method of the catalyst comprises the following steps: adding nickel nitrate into a hydrochloric acid solution, carrying out ultrasonic stirring in an ultrasonic instrument to completely dissolve the nickel nitrate, then adding carrier silicon dioxide, adding CaO into the solution which is pasty fluid, and placing the solution into an ultrasonic cleaning instrument to carry out ultrasonic stirring to fully dissolve the solution; then drying and roasting to obtain the catalyst; wherein: the molar ratio of the carrier silicon dioxide, the nickel nitrate and the hydrochloric acid solution is 1-1.02: 0.3-0.5: 1.05; the concentration of the hydrochloric acid solution is 15-30%.
Furthermore, the time of ultrasonic stirring in an ultrasonic instrument is 15 minutes, the time of ultrasonic placing in an ultrasonic cleaning instrument is 15 minutes, the roasting temperature is 550 ℃, and the roasting time is 4-5 hours.
Example 8
The catalyst preparation method is the same as that of example 7, (3) reverse osmosis: allowing the isopropanol after resin dehydration to pass through a reverse osmosis membrane, wherein the reverse osmosis pressure is 2.5Mpa, the permeation amount is 500L/h, and the circulation amount is controlled to be 800L/h; (4) high-temperature rectification: rectifying the isopropanol after reverse osmosis at high temperature, controlling the tower top temperature to be 82.5 ℃, the reflux ratio to be 1.2-2 and the temperature of condensed water to be less than 8 ℃. In this example, the yield of the isopropyl alcohol product was 96.9% and the purity was 99.3%.
Example 9
The catalyst preparation method is the same as that of example 7, (3) reverse osmosis: allowing the isopropanol after resin dehydration to pass through a reverse osmosis membrane, wherein the reverse osmosis pressure is 2.8Mpa, the permeation amount is 600L/h, and the circulation amount is controlled to be 900L/h; (4) high-temperature rectification: rectifying the isopropanol after reverse osmosis at high temperature, controlling the tower top temperature to be 82.5 ℃, the reflux ratio to be 1.2-2 and the temperature of condensed water to be less than 8 ℃. In this example, the yield of the rectified isopropanol product was 96.8%, and the purity was 99.4%.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, and that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A preparation method of high-purity isopropanol is characterized by comprising the following steps:
(1) crude isopropanol: the method comprises the following steps of taking acetone and hydrogen as raw materials, taking isopropanol as a solvent, wherein the mixture of the raw materials and the solvent comprises, by weight, 10-80% of acetone and 20-90% of isopropanol, and the raw materials and the catalyst are contacted at a reaction temperature of 100-160 ℃ and a reaction pressure of 1.0-5.0 MPa to react to generate the isopropanol, wherein the catalyst comprises the following components in percentage by weight: a) 40-97.5 parts of silicon dioxide carrier which is treated by acid, and b) 0.5-60 parts of nickel element or oxide thereof loaded on the silicon dioxide carrier, c) 3.0-15.0% of at least one of MgO, BaO or CaO;
(2) resin dehydration: enabling the prepared isopropanol to flow through the water-absorbing resin at a constant flow rate, and controlling the water content of the isopropanol to be reduced to below 20 ppm;
(3) reverse osmosis: enabling isopropanol after resin dehydration to pass through a reverse osmosis membrane, wherein the reverse osmosis pressure is 2.0-2.8Mpa, the permeability is 400-900L/h, and the circulation amount is controlled to be 700-900L/h;
(4) high-temperature rectification: rectifying the isopropanol subjected to reverse osmosis at high temperature, controlling the temperature of the top of the tower to be 82.0 +/-0.5 ℃, the reflux ratio to be 1.2-2, the temperature of condensed water to be less than 4-8 ℃, controlling the concentration of anions in the isopropanol after rectification at high temperature to be below 100ppb, and controlling the concentration of single cations to be below 1 ppb;
(5) and canning the rectified high-purity isopropanol.
2. The method according to claim 1, wherein the mixture of the raw material and the solvent contains 25.0 to 70.0% by weight of acetone and 30.0 to 65.0% by weight of isopropyl alcohol.
3. The method according to claim 1, wherein at least one selected from the group consisting of MgO, BaO and CaO is used in an amount of 5.0 to 10.0% by weight.
4. The method for preparing high-purity isopropanol according to claim 1, wherein the water-absorbent resin in step (2) is a polyacrylic acid-based water-absorbent resin.
5. The method for preparing high-purity isopropanol according to claim 1, wherein the method for preparing the catalyst comprises: adding nickel nitrate into a hydrochloric acid solution, carrying out ultrasonic stirring in an ultrasonic instrument to completely dissolve the nickel nitrate, then adding carrier silicon dioxide, adding at least one of MgO, BaO or CaO into the solution which is pasty fluid, and placing the solution in an ultrasonic cleaning instrument for ultrasonic stirring to completely dissolve the solution; then drying and roasting to obtain the catalyst; wherein: the molar ratio of the carrier silicon dioxide, the nickel nitrate and the hydrochloric acid solution is 1-1.02: 0.3-0.5: 1.05; the concentration of the hydrochloric acid solution is 15-30%.
6. The method for preparing high-purity isopropanol as claimed in claim 5, wherein the time of ultrasonic stirring in an ultrasonic instrument is 13-17 minutes, the time of ultrasonic cleaning in an ultrasonic cleaning instrument is 13-17 minutes, the roasting temperature is 450-550 ℃, and the roasting time is 4-5 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023102727A1 (en) * | 2021-12-07 | 2023-06-15 | 晶瑞电子材料股份有限公司 | Method for producing ultra-high purity isopropanol by using resin purification method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023102727A1 (en) * | 2021-12-07 | 2023-06-15 | 晶瑞电子材料股份有限公司 | Method for producing ultra-high purity isopropanol by using resin purification method |
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Application publication date: 20210226 |