CN109824498B - Diacetone alcohol continuous production device and production process - Google Patents
Diacetone alcohol continuous production device and production process Download PDFInfo
- Publication number
- CN109824498B CN109824498B CN201811575780.7A CN201811575780A CN109824498B CN 109824498 B CN109824498 B CN 109824498B CN 201811575780 A CN201811575780 A CN 201811575780A CN 109824498 B CN109824498 B CN 109824498B
- Authority
- CN
- China
- Prior art keywords
- tower
- reaction
- communicated
- temperature
- light component
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a diacetone alcohol continuous high-efficiency production device and a production process, the device comprises a reaction tower, the middle part of the reaction tower is provided with a feed inlet for inputting acetone, the bottom of the reaction tower is communicated with a light component removal tower, the bottom of the light component removal tower is communicated with a refining tower, the top of the refining tower is communicated with a first tower top condenser, the first condenser is communicated with a first tower top buffer tank, the first tower top buffer tank outputs finished diacetone alcohol, the middle part of the reaction tower is provided with a liquid distributor, a first reaction area solid alkaline catalyst is stacked below the liquid distributor inside the reaction tower, a second reaction area solid alkaline catalyst is stacked above the liquid distributor, and the stacking density and the stacking height of the first solid alkaline catalyst are smaller than those of the second solid alkaline catalyst. The production process is carried out by using the production device. The continuous efficient production device and the production process for diacetone alcohol have the characteristics of high product purity, high raw material conversion rate, high continuous degree and low cost.
Description
Technical Field
The invention relates to the technical field of diacetone alcohol, and particularly relates to a diacetone alcohol continuous efficient production device and a diacetone alcohol continuous efficient production process.
Background
Diacetone alcohol, also known as diacetone alcohol, is a two-molecule condensation product of acetone, is a colorless liquid, has a slight peppermint odor, is an important medium-boiling point solvent (166 ℃), and is also an important raw material and an intermediate for organic synthesis. The diacetone alcohol can be used as a solvent for dissolving oil, wax, natural resin, nitrocellulose, polymethyl methacrylate, polystyrene, dye and the like, and can be used as an intermediate for preparing important chemical products such as methyl isobutyl ketone, methyl pentadiene, isophorone and the like. The world market demand for this product also shows a rapidly increasing trend.
In response to the demand for diacetone alcohol, chinese patent No. CN1787986A discloses a method for producing diacetone alcohol capable of long-term operation, which relates to a method for producing diacetone alcohol from acetone in the presence of a solid basic catalyst containing at least (i) a metal hydroxide selected from an alkali metal hydroxide and an alkaline earth metal hydroxide and (ii) a binder, characterized in that as the solid basic catalyst, a solid basic catalyst having a pore volume of 1.8ml/g and a pore diameter of 0.01 to 1 μm is used. However, it must be seen that the scheme focuses on the introduction of the preparation of the composite catalyst for synthesizing diacetone alcohol, the reaction rate and the raw material conversion rate are not obviously improved in the reaction process route, the single-pass conversion rate within 48 hours is only 12% -15%, and the reaction period is longer.
The synthesis method and the process flow reported in the related documents and patents at present also relate to the defects of complex catalyst preparation, short service life, low yield, frequent intermittent production and the like.
Disclosure of Invention
The invention aims to provide a diacetone alcohol continuous high-efficiency production device and a production process, which have the characteristics of high product purity, high raw material conversion rate, high continuous degree and low cost.
The invention can be realized by the following technical scheme:
the invention discloses a diacetone alcohol continuous high-efficiency production device which comprises a reaction tower, wherein a feed inlet for inputting acetone is formed in the middle of the reaction tower, the bottom of the reaction tower is communicated with a light component removal tower, the bottom of the light component removal tower is communicated with a refining tower, the top of the refining tower is communicated with a first tower top condenser, the first tower top condenser is communicated with a first tower top buffer tank, the first tower top buffer tank outputs finished diacetone alcohol, a liquid distributor is arranged in the middle of the reaction tower, a first reaction area solid alkaline catalyst is stacked below the liquid distributor, a second reaction area solid alkaline catalyst is stacked above the liquid distributor, and the stacking density and the stacking height of the first reaction area solid alkaline catalyst are smaller than those of the second reaction area solid alkaline catalyst. . By adopting the scheme of the invention, the first reaction zone is positioned below the feed inlet and is closer to the tower kettle, the flow of the gas-liquid phase of the material in the first reaction zone is larger, the smaller catalyst stacking density is beneficial to the descending of the reaction liquid and the ascending of the evaporation gas of the tower kettle, and the risk of adverse working conditions such as flooding or tower body pressure rising is reduced. And the reflux liquid and the ascending gas in the second reaction zone have smaller flow, so that the catalyst with larger bulk density is selected to ensure the gas-liquid exchange and the full contact of the reaction materials and the catalyst, and the effective reaction can also be ensured.
And furthermore, the top of the reaction tower is communicated with a second tower top condenser, and the second tower top condenser is communicated with the reaction tower through a second tower top buffer tank.
And further, the top of the light component removal tower is communicated with a third tower top condenser, and the third tower top condenser is simultaneously communicated with the second tower top condenser and the refining tower through a third tower top buffer tank.
Further, the production device further comprises a light liquid collecting tank and a recovery tower, wherein the second tower top buffer tank and the third tower top buffer tank are communicated with the light liquid collecting tank, the light liquid collecting tank is communicated with the recovery tower, the top of the recovery tower is communicated with the second tower top condenser, and waste liquid is output from the bottom of the recovery tower.
Further, the bulk density of the solid alkaline catalyst in the first reaction zone is 200-500 kg/m3The stacking height is 1-4 m; the bulk density of the solid alkaline catalyst in the second reaction zone is 800-1500 kg/m3And the stacking height is 4-8 m.
Further, the height of the reaction tower is 10-15 m, and the feeding height of the raw material acetone is 6-8 m.
Further, the solid basic catalyst of the first reaction zone and the solid basic catalyst of the second reaction zone are both selected from one or a mixture of more than two of sodium hydroxide, potassium hydroxide, barium hydroxide, calcium hydroxide and anion exchange resin.
In another aspect of the invention, the production process adopting the production device is disclosed, the raw material acetone is precooled and then enters the middle part of the reaction tower, and then flows through the liquid distributor and then flows through the second reaction zone solid alkaline catalyst and the first solid alkaline oxidant which are piled up in two sections; controlling the temperature of a tower kettle of the reaction tower to be 80-130 ℃, distilling unreacted acetone in the tower kettle to the top of the reaction tower, condensing and refluxing, controlling the temperature of the top of the reaction tower to be 50-65 ℃, and condensing materials at the top of the reaction tower to be-10-25 ℃; pumping the tower kettle material of the reaction tower into the middle part of the light component removal tower through a pump, controlling the pressure of the light component removal tower to be 40-70 kpa, controlling the temperature of the kettle to be 100-140 ℃, controlling the temperature of the top of the tower to be 30-70 ℃, lightly condensing light components on the top of the tower, then feeding the light components into a second top of the tower buffer tank, controlling the temperature of a collecting solution to be 5-30 ℃, and enabling one part of the collecting solution to be the reflux of the light component removal tower and the other part of the collecting solution to be merged into a reflux line on the top of the reaction tower for continuous reaction; pumping the tower kettle materials of the light component removal tower into a refining tower through a pump, carrying out reduced pressure rectification under the pressure of 2-15 kpa, controlling the temperature of the tower kettle to be 90-150 ℃ and the temperature of the tower top to be 65-110 ℃, and collecting the finished products at the tower top.
Preferably, the precooling temperature of the raw material acetone is 15-30 ℃.
Preferably, the reflux ratio of the reaction tower is 2: 1-6: 1, and the temperature of a tower top condensate is-10-25 ℃;
preferably, the light component removal tower is a pressure reduction tower, the pressure of the light component removal tower is 50-80 kpa, the kettle temperature is 100-140 ℃, the tower top temperature is 30-70 ℃, and the reflux ratio is 2: 1-6: 1;
preferably, the refining tower is a decompression tower, the pressure is controlled to be 2-15 kpa, the tower top temperature is 65-110 ℃, the tower top temperature is 90-150 ℃, and the reflux ratio is 2: 1-4: 1.
The invention relates to a diacetone alcohol continuous high-efficiency production device, which has the following beneficial effects:
firstly, the product purity is high, and the finished product obtained by the device and the process is the target product diacetone alcohol with the content of more than 99.5 percent and has higher product purity;
secondly, the utilization rate of raw materials is high, and meanwhile, in the synthesis process, light impurities at the tops of the reaction tower and the light component removal tower are intermittently collected and periodically treated, and acetone in the light components is recovered to continuously participate in the reaction, so that the utilization rate of the raw materials is effectively improved;
thirdly, the degree of continuity is high, the whole production device is assembled by adopting a conventional chemical reaction tower, the reaction tower is communicated through a pipeline, and the reaction is circularly carried out, so that the continuity and the stability of the process synthesis are effectively ensured;
fourthly, the cost is low, the whole production process flow is simple, the acetone conversion rate is high, meanwhile, the energy consumption is low, and the equipment investment is low.
Drawings
FIG. 1 is a schematic composition diagram of a diacetone alcohol continuous high-efficiency production apparatus of the invention;
the reference numerals include: 1. A reaction tower; 2. A light component removal tower; 3. A refining tower; 4. A recovery tower; 5. A light liquid collecting tank; 6, a liquid distributor; 7. a precooler; 8. A second overhead condenser; 9. a third overhead condenser; 10. a first overhead condenser; 11. a second overhead buffer tank; 12. A third overhead surge tank; 13. a first overhead buffer tank; 14. a second reaction zone solid basic catalyst; 15. the first reaction zone is a solid basic catalyst.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the following detailed description is provided for the product of the present invention with reference to the examples.
As shown in figure 1, the invention discloses a diacetone alcohol continuous high-efficiency production device, which comprises a reaction tower 1, wherein the middle part of the reaction tower 1 is provided with a feed inlet for inputting acetone, the feed inlet is provided with a precooler 7, the bottom of the reaction tower 1 is communicated with a lightness-removing tower 2, the bottom of the lightness-removing tower 2 is communicated with a refining tower 3, the top of the refining tower 3 is communicated with a first tower top condenser 10, the first tower top condenser is communicated with a first tower top buffer tank 13, the first tower top buffer tank 13 outputs finished diacetone alcohol, the middle part of the reaction tower 1 is provided with a liquid distributor 6, a first reaction area solid alkaline catalyst is stacked below the liquid distributor 6 in the reaction tower 1, a second reaction area solid alkaline catalyst is stacked above the liquid distributor 6, and the stacking density and the stacking height of the first reaction area solid alkaline catalyst 15 are smaller than those of the second reaction area solid alkaline catalyst 14. The top of the reaction tower 1 is communicated with a second tower top condenser 8, and the second tower top condenser 8 is communicated with the reaction tower 1 through a second tower top buffer tank 11. The top of the light component removal tower 2 is communicated with a third tower top condenser 9, and the third tower top condenser 9 is simultaneously communicated with a second tower top condenser 8 and the refining tower 3 through a third tower top buffer tank 12. The production device further comprises a light liquid collecting tank 5 and a recovery tower 4, wherein a second tower top buffer tank 11 and a third tower top buffer tank 12 are communicated with the light liquid collecting tank, the light liquid collecting tank is communicated with the recovery tower 4, the top of the recovery tower 4 is communicated with a second tower top condenser 8, and waste liquid is output from the bottom of the recovery tower 4.
Further, the bulk density of the solid alkaline catalyst in the first reaction zone is 200-500 kg/m3The stacking height is 1-4 m; the bulk density of the solid alkaline catalyst in the second reaction zone is 800-1500 kg/m3And the stacking height is 4-8 m.
Further, the height of the reaction tower is 10-15 m, and the feeding height of the raw material acetone is 6-8 m.
Furthermore, the solid basic catalyst in the first reaction zone and the solid basic catalyst in the second reaction zone are both selected from one or a mixture of more than two of sodium hydroxide, potassium hydroxide, barium hydroxide, calcium hydroxide and anion exchange resin.
In another aspect of the invention, the production process adopting the production device is disclosed, the raw material acetone is precooled and then enters the middle part of the reaction tower, and then flows through the liquid distributor and then flows through the second reaction zone solid alkaline catalyst and the first solid alkaline oxidant which are piled up in two sections; controlling the temperature of a tower kettle of the reaction tower to be 80-130 ℃, distilling unreacted acetone in the tower kettle to the top of the reaction tower, condensing and refluxing, controlling the temperature of the top of the reaction tower to be 50-65 ℃, and condensing materials at the top of the reaction tower to be-10-25 ℃; pumping the tower kettle material of the reaction tower into the middle part of the light component removal tower through a pump, controlling the pressure of the light component removal tower to be 40-70 kpa, controlling the temperature of the kettle to be 100-140 ℃, controlling the temperature of the top of the tower to be 30-70 ℃, lightly condensing light components on the top of the tower, then feeding the light components into a second top of the tower buffer tank, controlling the temperature of a collecting solution to be 5-30 ℃, and enabling one part of the collecting solution to be the reflux of the light component removal tower and the other part of the collecting solution to be merged into a reflux line on the top of the reaction tower for continuous reaction; pumping the tower kettle materials of the light component removal tower into a refining tower through a pump, carrying out reduced pressure rectification under the pressure of 2-15 kpa, controlling the temperature of the tower kettle to be 90-150 ℃ and the temperature of the tower top to be 65-110 ℃, and collecting the finished products at the tower top.
Preferably, the precooling temperature of the raw material acetone is 15-30 ℃.
Preferably, the reflux ratio of the reaction tower is 2: 1-6: 1, and the temperature of a tower top condensate is-10-25 ℃;
preferably, the light component removal tower is a pressure reduction tower, the pressure of the light component removal tower is 50-80 kpa, the kettle temperature is 100-140 ℃, the tower top temperature is 30-70 ℃, and the reflux ratio is 2: 1-6: 1;
preferably, the refining tower is a decompression tower, the pressure is controlled to be 2-15 kpa, the tower top temperature is 65-110 ℃, the tower top temperature is 90-150 ℃, and the reflux ratio is 2: 1-4: 1.
In the efficient diacetone alcohol production device and the production process, the reflux ratio of the reaction tower and the light component removal tower is high, the discharge amount is small, the diacetone is periodically and intensively treated, and the diacetone is recovered for continuous reaction.
Example 1
The invention discloses a diacetone alcohol continuous high-efficiency production device which comprises a reaction tower, wherein a feed inlet for inputting acetone is formed in the middle of the reaction tower, a precooler is connected to the feed inlet, the bottom of the reaction tower is communicated with a light component removal tower, the bottom of the light component removal tower is communicated with a refining tower, the top of the refining tower is communicated with a first tower top condenser, the first tower top condenser is communicated with a first tower top buffer tank, the first tower top buffer tank outputs finished diacetone alcohol, a liquid distributor is arranged in the middle of the reaction tower, a first reaction area solid alkaline catalyst is stacked below the liquid distributor, a second reaction area solid alkaline catalyst is stacked above the liquid distributor, and the stacking density and the stacking height of the first reaction area solid alkaline catalyst are smaller than those of the second reaction area solid alkaline catalyst. The top of the reaction tower is communicated with a second tower top condenser, and the second tower top condenser is communicated with the reaction tower through a second tower top buffer tank. The top of the light component removal tower is communicated with a third tower top condenser, and the third tower top condenser is simultaneously communicated with the second tower top condenser and the refining tower through a third tower top buffer tank. The production device further comprises a light liquid collecting tank and a recovery tower, wherein the second tower top buffer tank and the third tower top buffer tank are communicated with the light liquid collecting tank, the light liquid collecting tank is communicated with the recovery tower, the top of the recovery tower is communicated with the second tower top condenser, and waste liquid is output from the bottom of the recovery tower.
In this example, the first reaction zone solid basic catalyst bulk density is 350kg/m3The stacking height is 1 m; the bulk density of the solid basic catalyst in the second reaction zone is 1500kg/m3The stacking height was 6 m. The height of the reaction tower is 10m, and the feeding height of the raw material acetone is 8 m. The solid alkaline catalyst in the first reaction zone and the solid alkaline catalyst in the second reaction zone are barium hydroxide.
In another aspect of the invention, the production process adopting the production device is disclosed, the raw material acetone is precooled and then enters the middle part of the reaction tower, and then flows through the liquid distributor and then flows through the second reaction zone solid alkaline catalyst and the first solid alkaline oxidant which are piled up in two sections; controlling the temperature of a tower kettle of the reaction tower to be 115 ℃, distilling unreacted acetone in the tower kettle to the top of the reaction tower, condensing and refluxing, controlling the temperature of the top of the reaction tower to be 50 ℃, and simultaneously condensing materials at the top of the reaction tower to be-25 ℃; pumping the tower kettle material of the reaction tower into the middle part of the light component removal tower through a pump, controlling the pressure of the light component removal tower to be 55kpa, the temperature of the kettle to be 100 ℃, the temperature of the tower top to be 70 ℃, condensing light components on the tower top to enter a second tower top buffer tank, controlling the collected liquid to be 17.5 ℃, enabling one part to be the reflux of the light component removal tower, and enabling one part to be merged into a reflux line on the top of the reaction tower for continuous reaction; pumping the tower bottom material of the light component removal tower into a refining tower by a pump, carrying out reduced pressure rectification under the pressure of 8.5kpa, controlling the tower bottom temperature to be 150 ℃, controlling the tower top temperature to be 85 ℃, and collecting the finished product at the tower top.
In this example, the precooling temperature of the acetone raw material was 15 ℃. The reflux ratio of the reaction tower is 6:1, and the temperature of the condensed liquid at the top of the tower is-17.5 ℃; the light component removal tower is a decompression tower, the pressure of the light component removal tower is 50kpa, the kettle temperature is 140 ℃, the temperature at the top of the tower is 50 ℃, and the reflux ratio is 4: 1; the refining tower is a pressure reducing tower, the pressure is controlled to be 15kpa, the tower top temperature is 110 ℃, the tower top temperature is 120 ℃, and the reflux ratio is 2: 1.
Through tests, the content of diacetone alcohol obtained in the embodiment is 99.5%, the alkali content of the waste liquid is 0.008%, the loss rate of the catalyst is 0.001%, and the conversion rate of the raw material is 95.2%.
Example 2
The invention discloses a diacetone alcohol continuous high-efficiency production device which comprises a reaction tower, wherein a feed inlet for inputting acetone is formed in the middle of the reaction tower, a precooler is connected to the feed inlet, the bottom of the reaction tower is communicated with a light component removal tower, the bottom of the light component removal tower is communicated with a refining tower, the top of the refining tower is communicated with a first tower top condenser, the first tower top condenser is communicated with a first tower top buffer tank, the first tower top buffer tank outputs finished diacetone alcohol, a liquid distributor is arranged in the middle of the reaction tower, a first reaction area solid alkaline catalyst is stacked below the liquid distributor, a second reaction area solid alkaline catalyst is stacked above the liquid distributor, and the stacking density and the stacking height of the first reaction area solid alkaline catalyst are smaller than those of the second reaction area solid alkaline catalyst. The top of the reaction tower is communicated with a second tower top condenser, and the second tower top condenser is communicated with the reaction tower through a second tower top buffer tank. The top of the light component removal tower is communicated with a third tower top condenser, and the third tower top condenser is simultaneously communicated with the second tower top condenser and the refining tower through a third tower top buffer tank. The production device further comprises a light liquid collecting tank and a recovery tower, wherein the second tower top buffer tank and the third tower top buffer tank are communicated with the light liquid collecting tank, the light liquid collecting tank is communicated with the recovery tower, the top of the recovery tower is communicated with the second tower top condenser, and waste liquid is output from the bottom of the recovery tower.
In this example, the first reaction zone solid basic catalyst bulk density is 500kg/m3The stacking height is 2.5 m; the bulk density of the solid basic catalyst in the second reaction zone is 800kg/m3And the stacking height is 8 m. The height of the reaction column was 12.5m and the feed height of the starting acetone was 6 m. The solid alkaline catalyst in the first reaction zone and the solid alkaline catalyst in the second reaction zone are both sodium hydroxide and potassium hydroxide.
In another aspect of the invention, the production process adopting the production device is disclosed, the raw material acetone is precooled and then enters the middle part of the reaction tower, and then flows through the liquid distributor and then flows through the second reaction zone solid alkaline catalyst and the first solid alkaline oxidant which are piled up in two sections; controlling the temperature of a tower kettle of the reaction tower to be 130 ℃, distilling unreacted acetone in the tower kettle to the top of the reaction tower, condensing and refluxing, controlling the temperature of the top of the reaction tower to be 57.5 ℃, and simultaneously condensing materials at the top of the reaction tower to be-10 ℃; pumping the tower kettle material of the reaction tower into the middle part of the light component removal tower through a pump, controlling the pressure of the light component removal tower at 70kpa, the temperature of the kettle at 120 ℃, the temperature of the tower top at 30 ℃, condensing light components on the tower top, then feeding the light components into a second tower top buffer tank, controlling the collected liquid at 30 ℃, wherein one part of the light components is reflux of the light component removal tower, and the other part of the light components is merged into a reflux line on the top of the reaction tower for continuous reaction; pumping the tower bottom material of the light component removal tower into a refining tower by a pump, carrying out reduced pressure rectification under 8.5kpa, controlling the tower bottom temperature to be 90 ℃, controlling the tower top temperature to be 110 ℃, and collecting the finished product at the tower top.
In this example, the precooling temperature of the acetone raw material was 22.5 ℃. The reflux ratio of the reaction tower is 4:1, and the temperature of the condensed liquid at the top of the tower is 25 ℃; the light component removal tower is a decompression tower, the pressure of the light component removal tower is 65kpa, the kettle temperature is 100 ℃, the tower top temperature is 70 ℃, and the reflux ratio is 2: 1; the refining tower is a vacuum tower, the pressure is controlled to be 8kpa, the tower top temperature is 65 ℃, the tower top temperature is 150 ℃, and the reflux ratio is 6: 1.
Through tests, the content of diacetone alcohol obtained in the embodiment is 99.7%, the alkali content of the waste liquid is 0.01%, and the loss rate of the catalyst is as follows: 0.002%, and the conversion rate of the raw material is 98.0%.
Example 3
The invention discloses a diacetone alcohol continuous high-efficiency production device which comprises a reaction tower, wherein a feed inlet for inputting acetone is formed in the middle of the reaction tower, a precooler is connected to the feed inlet, the bottom of the reaction tower is communicated with a light component removal tower, the bottom of the light component removal tower is communicated with a refining tower, the top of the refining tower is communicated with a first tower top condenser, the first tower top condenser is communicated with a first tower top buffer tank, the first tower top buffer tank outputs finished diacetone alcohol, a liquid distributor is arranged in the middle of the reaction tower, a first reaction area solid alkaline catalyst is stacked below the liquid distributor, a second reaction area solid alkaline catalyst is stacked above the liquid distributor, and the stacking density and the stacking height of the first reaction area solid alkaline catalyst are smaller than those of the second reaction area solid alkaline catalyst. The top of the reaction tower is communicated with a second tower top condenser, and the second tower top condenser is communicated with the reaction tower through a second tower top buffer tank. The top of the light component removal tower is communicated with a third tower top condenser, and the third tower top condenser is simultaneously communicated with the second tower top condenser and the refining tower through a third tower top buffer tank. The production device further comprises a light liquid collecting tank and a recovery tower, wherein the second tower top buffer tank and the third tower top buffer tank are communicated with the light liquid collecting tank, the light liquid collecting tank is communicated with the recovery tower, the top of the recovery tower is communicated with the second tower top condenser, and waste liquid is output from the bottom of the recovery tower.
In this example, the first reaction zone solid basic catalyst bulk density is 200kg/m3The stacking height is 4 m; the bulk density of the solid basic catalyst in the second reaction zone is 1150kg/m3And the stacking height is 5 m. The height of the reaction tower is 15m, and the feeding height of the raw material acetone is 7 m. The solid basic catalyst in the first reaction area and the solid basic catalyst in the second reaction area are anion exchange resin.
In another aspect of the invention, the production process adopting the production device is disclosed, the raw material acetone is precooled and then enters the middle part of the reaction tower, and then flows through the liquid distributor and then flows through the second reaction zone solid alkaline catalyst and the first solid alkaline oxidant which are piled up in two sections; controlling the temperature of a tower kettle of the reaction tower to be 80 ℃, distilling unreacted acetone in the tower kettle to the top of the reaction tower, condensing and refluxing, controlling the temperature of the top of the reaction tower to be 65 ℃, and simultaneously condensing materials at the top of the reaction tower to be-17.5 ℃; pumping the tower kettle material of the reaction tower into the middle part of the light component removal tower through a pump, controlling the pressure of the light component removal tower to be 40kpa, the temperature of the kettle to be 140 ℃, the temperature of the tower top to be 50 ℃, condensing light components on the tower top, then entering a second tower top buffer tank, controlling the collected liquid to be 5 ℃, refluxing a part of the light component removal tower, and merging a part of the light component removal tower into a reflux line on the top of the reaction tower for continuous reaction; pumping the tower bottom material of the light component removal tower into a refining tower by a pump, carrying out reduced pressure rectification under 15kpa, controlling the tower bottom temperature to be 120 ℃, controlling the tower top temperature to be 65 ℃, and collecting the finished product at the tower top.
In this example, the precooling temperature of the acetone raw material was 30 ℃. The reflux ratio of the reaction tower is 2:1, and the temperature of the condensed liquid at the top of the tower is-10 ℃; the light component removal tower is a decompression tower, the pressure of the light component removal tower is 80kpa, the kettle temperature is 120 ℃, the top temperature of the tower is 30 ℃, and the reflux ratio is 6: 1; the refining tower is a pressure reducing tower, the pressure is controlled to be 2kpa, the tower top temperature is 86 ℃, the tower top temperature is 90 ℃, and the reflux ratio is 4: 1.
Through tests, the content of diacetone alcohol obtained in the embodiment is 99.6%, the alkali content of the waste liquid is 0.013%, and the catalyst loss rate: 0.003 percent and the conversion rate of the raw material is 98.4 percent.
Example 4
The invention discloses a diacetone alcohol continuous high-efficiency production device which comprises a reaction tower, wherein a feed inlet for inputting acetone is formed in the middle of the reaction tower, a precooler is connected to the feed inlet, the bottom of the reaction tower is communicated with a light component removal tower, the bottom of the light component removal tower is communicated with a refining tower, the top of the refining tower is communicated with a first tower top condenser, the first tower top condenser is communicated with a first tower top buffer tank, the first tower top buffer tank outputs finished diacetone alcohol, a liquid distributor is arranged in the middle of the reaction tower, a first reaction area solid alkaline catalyst is stacked below the liquid distributor, a second reaction area solid alkaline catalyst is stacked above the liquid distributor, and the stacking density and the stacking height of the first reaction area solid alkaline catalyst are smaller than those of the second reaction area solid alkaline catalyst. The top of the reaction tower is communicated with a second tower top condenser, and the second tower top condenser is communicated with the reaction tower through a second tower top buffer tank. The top of the light component removal tower is communicated with a third tower top condenser, and the third tower top condenser is simultaneously communicated with the second tower top condenser and the refining tower through a third tower top buffer tank. The production device further comprises a light liquid collecting tank and a recovery tower, wherein the second tower top buffer tank and the third tower top buffer tank are communicated with the light liquid collecting tank, the light liquid collecting tank is communicated with the recovery tower, the top of the recovery tower is communicated with the second tower top condenser, and waste liquid is output from the bottom of the recovery tower.
In this example, the first reaction zone solid basic catalyst bulk density is 400kg/m3The stacking height is 2 m; the bulk density of the solid alkaline catalyst in the second reaction zone is 1200kg/m3And the stacking height is 5 m. The height of the reaction column was 14m and the feed height of the starting acetone was 6 m. The solid basic catalyst in the first reaction zone is anion exchange resin; the solid alkaline catalyst in the second reaction zone is sodium hydroxide, potassium hydroxide, barium hydroxide and calcium hydroxide.
In another aspect of the invention, the production process adopting the production device is disclosed, the raw material acetone is precooled and then enters the middle part of the reaction tower, and then flows through the liquid distributor and then flows through the second reaction zone solid alkaline catalyst and the first solid alkaline oxidant which are piled up in two sections; controlling the temperature of a tower kettle of the reaction tower to be 120 ℃, distilling unreacted acetone in the tower kettle to the top of the reaction tower, condensing and refluxing, controlling the temperature of the top of the reaction tower to be 55 ℃, and simultaneously condensing materials at the top of the reaction tower to be 15 ℃; pumping the tower kettle material of the reaction tower into the middle part of the light component removal tower through a pump, controlling the pressure of the light component removal tower to be 50kpa, the temperature of the kettle to be 130 ℃, the temperature of the tower top to be 40 ℃, condensing light components on the tower top, then entering a second tower top buffer tank, controlling the collected liquid to be 20 ℃, refluxing a part of the light component removal tower, and merging a part of the light component removal tower into a reflux line on the top of the reaction tower for continuous reaction; pumping the tower bottom material of the light component removal tower into a refining tower by a pump, carrying out reduced pressure rectification under the condition of 5kpa, controlling the tower bottom temperature to be 130 ℃, controlling the tower top temperature to be 70 ℃, and collecting a finished product at the tower top.
In this example, the precooling temperature of the acetone raw material was 20 ℃. The reflux ratio of the reaction tower is 3:1, and the temperature of the condensed liquid at the top of the tower is-15 ℃; the light component removal tower is a decompression tower, the pressure of the light component removal tower is 60kpa, the kettle temperature is 120 ℃, the temperature at the top of the tower is 50 ℃, and the reflux ratio is 3: 1; the refining tower is a pressure reducing tower, the pressure is controlled to be 6kpa, the tower top temperature is 90 ℃, the tower top temperature is 100 ℃, and the reflux ratio is 3: 1.
Through tests, the content of diacetone alcohol obtained in the embodiment is 99.7%, the alkali content of the waste liquid is 0.014%, and the catalyst loss rate: 0.005% and the conversion of the raw material was 97.2%.
Example 5
The invention discloses a diacetone alcohol continuous high-efficiency production device which comprises a reaction tower, wherein a feed inlet for inputting acetone is formed in the middle of the reaction tower, a precooler is connected to the feed inlet, the bottom of the reaction tower is communicated with a light component removal tower, the bottom of the light component removal tower is communicated with a refining tower, the top of the refining tower is communicated with a first tower top condenser, the first tower top condenser is communicated with a first tower top buffer tank, the first tower top buffer tank outputs finished diacetone alcohol, a liquid distributor is arranged in the middle of the reaction tower, a first reaction area solid alkaline catalyst is stacked below the liquid distributor, a second reaction area solid alkaline catalyst is stacked above the liquid distributor, and the stacking density and the stacking height of the first reaction area solid alkaline catalyst are smaller than those of the second reaction area solid alkaline catalyst. The top of the reaction tower is communicated with a second tower top condenser, and the second tower top condenser is communicated with the reaction tower through a second tower top buffer tank. The top of the light component removal tower is communicated with a third tower top condenser, and the third tower top condenser is simultaneously communicated with the second tower top condenser and the refining tower through a third tower top buffer tank. The production device further comprises a light liquid collecting tank and a recovery tower, wherein the second tower top buffer tank and the third tower top buffer tank are communicated with the light liquid collecting tank, the light liquid collecting tank is communicated with the recovery tower, the top of the recovery tower is communicated with the second tower top condenser, and waste liquid is output from the bottom of the recovery tower.
In this example, the first reaction zone solid basic catalyst bulk density is 300kg/m3The stacking height is 3 m; the bulk density of the solid basic catalyst in the second reaction zone is 900kg/m3The stacking height was 6 m. The height of the reaction tower is 12m, and the feeding height of the raw material acetone is 8 m. The solid alkaline catalyst in the first reaction zone is sodium hydroxide, potassium hydroxide, barium hydroxide and calcium hydroxide; the solid alkaline catalyst in the second reaction zone is sodium hydroxide, potassium hydroxide or barium hydroxide.
In another aspect of the invention, the production process adopting the production device is disclosed, the raw material acetone is precooled and then enters the middle part of the reaction tower, and then flows through the liquid distributor and then flows through the second reaction zone solid alkaline catalyst and the first solid alkaline oxidant which are piled up in two sections; controlling the temperature of a tower kettle of the reaction tower to be 110 ℃, distilling unreacted acetone in the tower kettle to the top of the reaction tower, condensing and refluxing, controlling the temperature of the top of the reaction tower to be 60 ℃, and simultaneously condensing materials at the top of the reaction tower to be 5 ℃; pumping the tower kettle material of the reaction tower into the middle part of the light component removal tower through a pump, controlling the pressure of the light component removal tower to be 60kpa, the temperature of the kettle to be 110 ℃, the temperature of the tower top to be 50 ℃, condensing light components on the tower top, then entering a second tower top buffer tank, controlling the collected liquid to be 20 ℃, refluxing a part of the light component removal tower, and merging a part of the light component removal tower into a reflux line on the top of the reaction tower for continuous reaction; pumping the tower bottom material of the light component removal tower into a refining tower by a pump, carrying out reduced pressure rectification under 11kpa, controlling the tower bottom temperature to be 110 ℃, controlling the tower top temperature to be 100 ℃, and collecting a finished product at the tower top.
In this embodiment, the pre-cooling temperature of the acetone raw material is 15-30 ℃. The reflux ratio of the reaction tower is 4:1, and the temperature of the condensed liquid at the top of the tower is 8 ℃; the light component removal tower is a decompression tower, the pressure of the light component removal tower is 70kpa, the kettle temperature is 120 ℃, the tower top temperature is 60 ℃, and the reflux ratio is 5: 1; the refining tower is a vacuum tower, the pressure is controlled to be 12kpa, the tower top temperature is 90 ℃, the tower top temperature is 130 ℃, and the reflux ratio is 3: 1.
Through tests, the content of diacetone alcohol obtained in the embodiment is 99.6%, the alkali content of the waste liquid is 0.009%, and the catalyst loss rate: 0.0013 percent.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; as will be readily apparent to those skilled in the art from the disclosure herein, the present invention may be practiced without these specific details; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention; meanwhile, any changes, modifications, and evolutions of the equivalent changes of the above embodiments according to the actual techniques of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. The utility model provides a diacetone alcohol serialization apparatus for producing, includes the reaction column, the reaction column middle part is equipped with the feed inlet that supplies acetone input, its characterized in that: the reactor comprises a reaction tower, a light component removing tower, a refining tower, a first tower top condenser, a first tower top buffer tank, a second reaction zone solid alkaline catalyst, a liquid distributor and a second reaction zone solid alkaline catalyst, wherein the bottom of the reaction tower is communicated with the light component removing tower, the top of the refining tower is communicated with the first tower top condenser, the first tower top condenser is communicated with the first tower top buffer tank, the first tower top buffer tank outputs finished product diacetone alcohol, the middle of the reaction tower is provided with the liquid distributor, the liquid distributor is arranged inside the reaction tower, the lower part of the liquid distributor is piled with the first reaction zone solid alkaline catalyst, the upper part of the liquid distributor is piled with the second reaction zone solid alkaline catalyst, and the piling density and the piling height of the first reaction zone solid alkaline catalyst are less than the second reaction zone solid alkaline catalyst.
2. The diacetone alcohol continuous production apparatus according to claim 1, wherein: the top of the reaction tower is communicated with a second tower top condenser, and the second tower top condenser is communicated with the reaction tower through a second tower top buffer tank.
3. The diacetone alcohol continuous production apparatus according to claim 2, wherein: and the top of the light component removal tower is communicated with a third tower top condenser, and the third tower top condenser is simultaneously communicated with a second tower top condenser and the refining tower through a third tower top buffer tank.
4. The continuous diacetone alcohol production apparatus according to claim 3, wherein: the production device further comprises a light liquid collecting tank and a recovery tower, wherein the second tower top buffer tank and the third tower top buffer tank are communicated with the light liquid collecting tank, the light liquid collecting tank is communicated with the recovery tower, the top of the recovery tower is communicated with the second tower top condenser, and waste liquid is output from the bottom of the recovery tower.
5. The continuous diacetone alcohol production apparatus according to claim 4, wherein: the bulk density of the solid basic catalyst in the first reaction zone is 200-500 kg/m3The stacking height is 1-4 m; the bulk density of the solid alkaline catalyst in the second reaction zone is 800-1500 kg/m3And the stacking height is 4-8 m.
6. The continuous diacetone alcohol production apparatus according to claim 4 or 5, wherein: the height of the reaction tower is 10-15 m, and the feeding height of the raw material acetone is 6-8 m.
7. The continuous diacetone alcohol production apparatus according to claim 6, wherein: the solid basic catalyst in the first reaction zone and the solid basic catalyst in the second reaction zone are respectively selected from one or a mixture of more than two of sodium hydroxide, potassium hydroxide, barium hydroxide, calcium hydroxide and anion exchange resin.
8. A production process using the production apparatus as set forth in any one of claims 1 to 7, characterized in that: precooling a raw material acetone, then feeding the acetone into the middle part of a reaction tower, and uniformly flowing the acetone through a liquid distributor and a second reaction zone solid alkaline catalyst and a first reaction zone solid alkaline catalyst which are stacked in two sections;
controlling the temperature of a tower kettle of the reaction tower to be 80-130 ℃, distilling unreacted acetone in the tower kettle to the top of the reaction tower, condensing and refluxing, controlling the temperature of the top of the reaction tower to be 50-65 ℃, and condensing materials at the top of the reaction tower to be-10-25 ℃;
pumping the tower kettle material of the reaction tower into the middle part of the light component removal tower through a pump, controlling the pressure of the light component removal tower to be 40-70 kpa, controlling the temperature of the kettle to be 100-140 ℃, controlling the temperature of the top of the tower to be 30-70 ℃, lightly condensing light components on the top of the tower, then feeding the light components into a second top of the tower buffer tank, controlling the temperature of a collecting solution to be 5-30 ℃, and enabling one part of the collecting solution to be the reflux of the light component removal tower and the other part of the collecting solution to be merged into a reflux line on the top of the reaction tower for continuous reaction;
pumping the tower kettle materials of the light component removal tower into a refining tower through a pump, carrying out reduced pressure rectification under the pressure of 2-15 kpa, controlling the temperature of the tower kettle to be 90-150 ℃ and the temperature of the tower top to be 65-110 ℃, and collecting the finished products at the tower top.
9. The production process according to claim 8, wherein: the precooling temperature of the raw material acetone is 15-30 ℃.
10. The production process according to claim 9, characterized in that: the reflux ratio of the reaction tower is 2: 1-6: 1, and the temperature of a condensate at the top of the tower is-10-25 ℃;
the light component removing tower is a pressure reducing tower, the pressure of the light component removing tower is 50-80 kpa, the kettle temperature is 100-140 ℃, the temperature of the top of the tower is 30-70 ℃, and the reflux ratio is 2: 1-6: 1;
the refining tower is a decompression tower, the pressure is controlled to be 2-15 kpa, the tower top temperature is 65-110 ℃, the tower top temperature is 90-150 ℃, and the reflux ratio is 2: 1-4: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811575780.7A CN109824498B (en) | 2018-12-22 | 2018-12-22 | Diacetone alcohol continuous production device and production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811575780.7A CN109824498B (en) | 2018-12-22 | 2018-12-22 | Diacetone alcohol continuous production device and production process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109824498A CN109824498A (en) | 2019-05-31 |
| CN109824498B true CN109824498B (en) | 2021-12-14 |
Family
ID=66860219
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811575780.7A Active CN109824498B (en) | 2018-12-22 | 2018-12-22 | Diacetone alcohol continuous production device and production process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109824498B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110496414B (en) * | 2019-09-19 | 2021-04-27 | 福州大学 | Continuous reaction rectification equipment for synthesizing diacetone alcohol and process thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1772722A (en) * | 2004-11-11 | 2006-05-17 | 中国石化上海石油化工股份有限公司 | Methyl heptenone preparing and refining process |
| CN1787986A (en) * | 2003-05-15 | 2006-06-14 | 三菱化学株式会社 | Process for producing diacetone alcohol |
| CN101367041A (en) * | 2008-09-26 | 2009-02-18 | 华东理工大学 | Preparation of solid base catalyst, uses of the same in hydroxide aldehyde condensation reaction |
| CN101659604A (en) * | 2009-07-14 | 2010-03-03 | 南京工程学院 | Method for preparing 4-methyl-4-hydroxyl-2-pentanone by using solid base as catalyst |
| CN102757327A (en) * | 2011-04-29 | 2012-10-31 | 中国石油化工股份有限公司 | Method for preparing diacetone alcohol by oxidizing acetone |
| CN203256179U (en) * | 2013-04-27 | 2013-10-30 | 江苏凯茂石化科技有限公司 | Technological equipment for processing methylisobutylketone |
| CN103435461A (en) * | 2013-07-24 | 2013-12-11 | 河北工业大学 | Production technology for isophorone |
| CN103467263A (en) * | 2013-09-13 | 2013-12-25 | 江苏焕鑫高新材料科技有限公司 | Preparation method of isophorone |
| CN103724172A (en) * | 2014-01-17 | 2014-04-16 | 天津市道福化工新技术开发有限公司 | Synthesis process of diacetone alcohol |
| CN104478683A (en) * | 2014-09-24 | 2015-04-01 | 浙江新化化工股份有限公司 | Synthetic method of 2-heptanone |
| CN106083544A (en) * | 2016-06-02 | 2016-11-09 | 中国化学赛鼎宁波工程有限公司 | Cyclohexanone is refined and cyclohexanol recoverying and utilizing method and system |
-
2018
- 2018-12-22 CN CN201811575780.7A patent/CN109824498B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1787986A (en) * | 2003-05-15 | 2006-06-14 | 三菱化学株式会社 | Process for producing diacetone alcohol |
| CN1772722A (en) * | 2004-11-11 | 2006-05-17 | 中国石化上海石油化工股份有限公司 | Methyl heptenone preparing and refining process |
| CN101367041A (en) * | 2008-09-26 | 2009-02-18 | 华东理工大学 | Preparation of solid base catalyst, uses of the same in hydroxide aldehyde condensation reaction |
| CN101659604A (en) * | 2009-07-14 | 2010-03-03 | 南京工程学院 | Method for preparing 4-methyl-4-hydroxyl-2-pentanone by using solid base as catalyst |
| CN102757327A (en) * | 2011-04-29 | 2012-10-31 | 中国石油化工股份有限公司 | Method for preparing diacetone alcohol by oxidizing acetone |
| CN203256179U (en) * | 2013-04-27 | 2013-10-30 | 江苏凯茂石化科技有限公司 | Technological equipment for processing methylisobutylketone |
| CN103435461A (en) * | 2013-07-24 | 2013-12-11 | 河北工业大学 | Production technology for isophorone |
| CN103467263A (en) * | 2013-09-13 | 2013-12-25 | 江苏焕鑫高新材料科技有限公司 | Preparation method of isophorone |
| CN103724172A (en) * | 2014-01-17 | 2014-04-16 | 天津市道福化工新技术开发有限公司 | Synthesis process of diacetone alcohol |
| CN104478683A (en) * | 2014-09-24 | 2015-04-01 | 浙江新化化工股份有限公司 | Synthetic method of 2-heptanone |
| CN106083544A (en) * | 2016-06-02 | 2016-11-09 | 中国化学赛鼎宁波工程有限公司 | Cyclohexanone is refined and cyclohexanol recoverying and utilizing method and system |
Non-Patent Citations (2)
| Title |
|---|
| 反应-蒸馏合成双丙酮醇工艺研究;田红丽等;《信阳师范学院学报》;20150731;第393-395页 * |
| 连续固定床反应器合成二丙酮醇的研究;周诗彪等;《精细化工中间体》;20051231;第35卷(第5期);第38-40页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109824498A (en) | 2019-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104355975B (en) | A kind of method of acetone two step synthesis methyl iso-butyl ketone (MIBK) | |
| CN1830934A (en) | Method for producing dimethyl ether using methanol as raw material | |
| CN112209808A (en) | Novel process for producing sodium methoxide | |
| CN103274913A (en) | Method and device for producing methyl isobutyl ketone | |
| CN109824498B (en) | Diacetone alcohol continuous production device and production process | |
| CN109748791B (en) | Energy-saving method for producing dimethyl adipate | |
| CN102115444B (en) | Process and device for continuously producing glyceryl triacetate | |
| CN103342642A (en) | Process for continuously producing dimethyl adipate through reaction-rectification method | |
| CN109748790B (en) | Method for producing dimethyl adipate | |
| CN108774100B (en) | Combined method for preparing methyl tert-butyl ether and isobutene from tert-butyl alcohol and methanol | |
| CN112537998B (en) | Process for producing neopentyl glycol by continuous catalytic hydrogenation | |
| CN115160106A (en) | Production device and method of sec-butyl alcohol | |
| CN102471194A (en) | Method and system for producing methanol and dimethyl ether | |
| CN108947774A (en) | A kind of method and device of separating isopropanol | |
| CN101550065B (en) | Energy-saving and water-saving type high-low pressure double-tower process for preparing dimethyl ether by rectifying methanol | |
| CN112479869B (en) | Method for rectifying dimethyl oxalate in coal chemical industry | |
| CN109646977B (en) | Reactive distillation coupling tower and application thereof in preparation of formic acid | |
| KR20000072037A (en) | Method and apparatus of methyl acetate hydrolysis | |
| CN201524434U (en) | Integrated evaporator for carbonylation acetic acid technology | |
| CN114853588B (en) | Separation process of supercritical synthetic butanone alcohol reaction liquid | |
| CN101429106A (en) | Low-energy consumption synthesis process for dimethyl ether | |
| CN101429105A (en) | Process for synthesis of with gas-phase methanol dehydration and used apparatus thereof | |
| CN209906679U (en) | Device for preparing methyl formate by catalytic distillation | |
| CN209778706U (en) | Continuous system for catalyzing esterification of low-boiling-point alcohol by solid acid | |
| CN115364504B (en) | System and method for separating acetaldehyde from diethyl ether |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 529080 Shi Heli (solvent factory), Jianghai Road, Waihai, Jiangmen City, Guangdong Province Applicant after: Qianhang Chemical Group Co., Ltd Address before: 529080 Shi Heli (solvent factory), Jianghai Road, Waihai, Jiangmen City, Guangdong Province Applicant before: Jiangmen Qianxin Chemical Development Co., Ltd |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220215 Address after: 519000 southwest of pingwan 1st Road, petrochemical zone, Gaolan Port Economic Zone, Zhuhai City, Guangdong Province Patentee after: Zhuhai Qianxin New Material Co.,Ltd. Address before: 529080 shiheli (solvent factory), Jianghai Road, Waihai, Jiangmen City, Guangdong Province Patentee before: Qianxin Chemical Group Co.,Ltd. |