CN115093318A - Process and device for producing isovaleric acid from isoamyl alcohol - Google Patents
Process and device for producing isovaleric acid from isoamyl alcohol Download PDFInfo
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- CN115093318A CN115093318A CN202210487914.XA CN202210487914A CN115093318A CN 115093318 A CN115093318 A CN 115093318A CN 202210487914 A CN202210487914 A CN 202210487914A CN 115093318 A CN115093318 A CN 115093318A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/02—Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
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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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- 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
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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
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/295—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with inorganic bases, e.g. by alkali fusion
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
Abstract
The invention relates to a method and a device for producing isovaleric acid by using isoamyl alcohol, which mainly solve the problems of serious three wastes and low yield in the isovaleric acid synthesis process. The high-purity isovaleric acid is synthesized through three steps of an oxidation process, an acidification process and a rectification process. The process improves the reaction rate and the conversion rate of the process by using the high-selectivity white oil as a reaction solvent; meanwhile, the temperature is controlled through the heat conduction oil, and the nitrogen input, the hydrogen discharge, the raw material and catalytic addition speed and the product discharge speed are automatically controlled, so that a safe production environment is obtained, and the production efficiency and the product quality are greatly improved. Therefore, the method and the device for producing the isovaleric acid by using the isoamyl alcohol can effectively improve the stability and the yield of the production process of the isooctanoic acid, and have safe and stable equipment and high environmental protection.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of fine chemical engineering, and particularly relates to a method and a device for producing isovaleric acid by using isoamyl alcohol, which is a method for producing isovaleric acid in the perfume industry.
[ background of the invention ]
The isovaleric acid is used as a basic raw material for synthesizing spices and food additives, can produce a large amount of isovaleric acid ester and derivatives thereof, can be used as spices and food additives, and the production of isovaleric acid by using biological fermentation isoamylol as a raw material meets the natural equivalent requirements of the American FDA, and the demand is increased year by year. The biomass isoamyl alcohol is widely present in fusel oil which is a main byproduct of the method for preparing the ethanol by the grain crop fermentation method and accounts for about 50 percent of the total amount of the fusel oil. Therefore, a process route and a device for efficiently producing isovaleric acid by using biomass isoamyl alcohol as a raw material are urgently needed to be developed, the ethanol byproduct fusel oil is reasonably utilized, the resource waste is avoided, and high-added-value fine chemicals are generated.
Patent CN201610715638A discloses a method for preparing lower alcohols. The patent utilizes low carbon alcohol, water and urea to be stirred and mixed, and then hydrogen peroxide is dripped to carry out oxidation reaction, so that the process has little pollution and good environmental benefit. But the reaction is violent, the control is difficult, and the industrial operation is not available at home at present.
Patent CN201710216243A discloses a method for synthesizing isovaleric acid, a drug intermediate. In the patent, 1-chloro-3-isopropyl acetone and dimethyl carbonate are used as raw materials, manganese chloride and potassium chloride are used as catalysts, and after the reaction is finished, potassium hydrogen sulfate is used for adjusting the pH value and methyl carbitol is used for washing. The production process is complex, a large amount of waste liquid can be generated, the environmental protection pressure is high, and the yield is not ideal.
Patent CN201810009043A discloses a bacillus and its method for producing isovaleric acid. The patent reasonably utilizes waste produced in the tobacco industry as a fermentation culture medium to synthesize the isovaleric acid, but the strain is easily influenced by environmental factors, and the industrial production is not realized at present.
In conclusion, the existing method for producing the isovaleric acid by using the isoamyl alcohol has the disadvantages of complex process, serious three wastes and low yield; some methods have not been industrialized, so it is necessary to develop a suitable synthesis method, which is of great significance for further improving the quality and yield of the product and carrying out industrial production.
[ summary of the invention ]
In order to overcome the defects of the prior art, the invention provides a method and a device for producing isovaleric acid by using isoamyl alcohol, and solves the problems of violent reaction, difficult control, serious pollution, low product yield and the like in the prior production technology.
In order to realize the purpose of the invention, the invention adopts the following technical scheme: a production device for producing isovaleric acid from isoamyl alcohol is characterized in that the device is provided with an oxidation device, an acidification device and a rectification device which are connected in sequence according to working procedures. The oxidation device comprises a reflux high-pressure oxidation kettle, an external heating device of the reflux high-pressure oxidation kettle is connected with a heat conduction oil mechanism, and the reflux high-pressure oxidation kettle is respectively connected with a nitrogen supply pipeline, a fresh water input pipeline, an isoamyl alcohol pipeline, a white oil pipeline, a hydrogen recovery pipeline and a catalyst input pipeline; reflux high-pressure oxidation kettle connect through sodium iso valerate discharge line the acidizing device, the acidizing device include the acidizing cauldron, the acidizing cauldron pass through the pipeline and connect fresh water tank and sulfuric acid tank respectively, the acidizing cauldron still be connected with cooling circulation water system and crude isovaleric acid discharge line, the acidizing cauldron in be provided with rabbling mechanism, crude isovaleric acid discharge line connect the rectifier unit.
An isoamylol pump, an automatic cut-off valve and a flowmeter are arranged between the reflux high-pressure oxidation kettle and the isoamylol tank; a white oil pump, an automatic cut-off valve and a flowmeter are arranged between the reflux high-pressure oxidation kettle and the white oil tank; a pressure transmitter and a regulating valve are arranged on the hydrogen recovery pipeline; the isoamylol recovery tank is connected with an emptying tank; the white oil tank is connected with an isoamylol recovery tank, and the white oil recovery tank is connected with an emptying tank.
A water injection pump, an automatic cut-off valve and a flowmeter are arranged on a pipeline between the acidification kettle and the fresh water tank; a sulfuric acid pump, a regulating valve and a flowmeter are arranged on a pipeline between the acidification kettle and the sulfuric acid tank; a crude isovaleric acid discharge pipeline is provided with a crude isovaleric acid pump.
The rectifying device comprises a condenser and a reboiler, and the tower bottom is connected with an isovaleric acid storage tank.
The technical scheme provided by the invention has the following beneficial effects:
1. the invention adopts the white oil as the reaction solvent, so that the reaction system can be quickly raised to 240, the white oil has emulsification effect at high temperature, the caustic soda melting and isoamylol dehydrogenation reaction speeds are increased, and the selectivity and the reaction quality conversion of the method are higher than those of the similar processes.
2. White oil is used as a solvent, and the reaction materials are in a liquid flow state in a cooling state, so that the defect that solid salt is not easy to unload in the cooling process in the solvent-free reaction is avoided, and the requirement on reaction equipment is lowered.
3. The temperature control is carried out through the heat conduction oil, so that the whole course of the oxidation process is at the optimal reaction temperature, and the nitrogen input, the hydrogen discharge, the raw material and catalytic addition speed and the product discharge speed are automatically controlled, so that the safe environment and the fastest reaction are obtained, and the production efficiency and the product quality are greatly improved.
In conclusion, the method and the device for producing the isovaleric acid by using the isoamyl alcohol can improve the stability and the yield of the production process of the isooctanoic acid, and have safe and stable equipment and high environmental protection.
[ description of the drawings ]
FIG. 1 is a flow chart of a production process for producing isovaleric acid from isoamyl alcohol.
Included in figure 1 are: 1. an isoamyl alcohol tank; 2. an oxidation kettle; 3. a white oil pipe; 4. a fresh water pipeline; 5.N 2 (ii) a 6, a catalyst pipeline; 7. a heat conductive oil conduit; 8. a hydrogen gas conduit; 9. an sodium iso-valerate pipeline; 10. an acidification tank; 11. a fresh water pipeline; 12. sulfuric acid pipeline(ii) a 13. A circulating water pipeline; 14. a white oil extraction pipeline; 15. a wastewater treatment tank; 16. an isovaleric acid crude product pipeline; 17. a storage tank for the crude isovaleric acid; 18. a rectification column; 19. a condenser; 20. a reboiler; 21. and (4) an isovaleric acid storage tank.
[ detailed description ] embodiments
The following further description, taken in conjunction with the accompanying drawings, is not intended to limit the scope of the invention
A production process for producing isovaleric acid from isoamyl alcohol is characterized by comprising the following steps:
the first step is as follows: oxidation process
Quantitative white oil, flake caustic soda, catalyst and isoamylol are put into a reflux high-pressure oxidation kettle, stirred and heated through heat conduction oil to control the temperature of the reflux high-pressure oxidation kettle within a certain range, and then the reflux high-pressure oxidation kettle is started. After the feeding is finished, residual oxygen in the kettle is replaced by nitrogen, and the oxidation kettle is closed. Stirring is started, the reaction is started, and H is continuously generated in the process 2 The pressure and the temperature of the oxidation kettle are gradually increased, and when the temperature reaches 240 and the pressure reaches 1.8MPa, H is discharged 2 This stage ensures H 2 The discharge amount and the generation amount are approximately equal, and the pressure is stabilized at 1.8MPa to ensure that the reaction is efficiently and fully carried out. When the reaction is near the end, H 2 Little production, pressure maintaining for 30min to ensure complete reaction, and pressure relief. After the pressure relief is finished, adding a certain amount of water to discharge residual H in the oxidation kettle 2 And closing the oxidation kettle after the reaction is finished, wherein the temperature in the oxidation kettle is very high, then generating a large amount of steam, and finally pressing the reaction intermediate sodium isovalerate mixed solution to the acidification kettle when the pressure reaches 0.6MPa, so that the first-step reaction is finished.
The second step is that: acidification step
Firstly, pressing the mixed solution of sodium isovalerate reacted in the oxidation device to an acidification kettle, and adding quantitative pure water. Then, slowly adding sulfuric acid at a constant speed, releasing heat in the process, opening cooling circulating water, controlling the temperature of an acidification kettle to be below 100, gradually reducing the pH value of the material along with the reaction, and ending the acid addition when the pH value reaches a set value of pH 3.0. Standing for a period of time to allow the crude isovaleric acid and the sodium sulfate solution to be layered, finally discharging the sodium sulfate solution to a wastewater treatment tank, and discharging the crude isovaleric acid to an intermediate storage tank.
The third step: rectification step
Firstly, conveying the crude isovaleric acid in an intermediate storage tank into the rectifying tower through a pump, and introducing steam of 0.5-0.8 MPa (gauge pressure) into a reboiler at the bottom of the tower for heating. In the rectifying tower, because the boiling point of water is low, the water is continuously enriched in a gas phase and rises to the tower top, and the boiling point of isovaleric acid is high, the isovaleric acid is continuously enriched in a liquid phase and falls to the tower bottom, and the isovaleric acid is extracted to an isovaleric acid storage tank through a liquid phase outlet at the tower bottom.
Claims (4)
1. A process and a device for producing isovaleric acid by using isoamyl alcohol are characterized in that the device for realizing the method mainly comprises the following parts: 1. an isoamyl alcohol tank; 2. an oxidation kettle; 3. a white oil pipe; 4. a fresh water pipeline; 5.N 2 (ii) a 6. A catalyst conduit; 7. a heat conductive oil pipeline; 8. a hydrogen gas conduit; 9. a sodium iso-valerate pipeline; 10. an acidification tank; 11. a fresh water pipeline; 12. a sulfuric acid pipeline; 13. a circulating water pipeline; 14. a white oil extraction pipeline; 15. a wastewater treatment tank; 16. an isovaleric acid crude product pipeline; 17. a storage tank for the crude isovaleric acid; 18. a rectification column; 19. a condenser; 20. a reboiler; 21. an isovaleric acid storage tank;
the method for carrying out the process for producing the isovaleric acid by the isoamylol by adopting the device comprises the following steps:
(1) oxidation process
Quantitative white oil, flake caustic soda, a catalyst and isoamylol are added into a reflux high-pressure oxidation kettle, stirred and heated by heat-conducting oil to control the temperature of the reflux high-pressure oxidation kettle within a certain range, and then the reflux high-pressure oxidation kettle is started; after the feeding is finished, residual oxygen in the clean kettle is replaced by nitrogen, the closed oxidation kettle is stirred, the reaction is started, and H is continuously generated in the process 2 The pressure and the temperature of the oxidation kettle are gradually increased, and H is discharged when the temperature reaches 240 ℃ and the pressure reaches 1.8MPa 2 This stage ensures H 2 The discharge amount and the generation amount are approximately equal, and the pressure is stabilized at 1.8MPa to ensure that the reaction is efficiently and fully carried out; when the reaction is near the end, H 2 The production amount is small, the pressure is maintained for a certain time of 30min, the reaction is thorough, and then the pressure is released; drain deviceAfter the pressure is finished, adding a certain amount of water, and discharging residual H in the oxidation kettle 2 Closing the oxidation kettle after the reaction is finished, ensuring that the temperature in the oxidation kettle is very high, then generating a large amount of steam, and finally pressing the mixed solution of sodium isovalerate serving as a reaction intermediate to the acidification kettle when the pressure reaches 0.6MPa, and finishing the reaction in the first step;
(2) acidification step
Firstly, pressing a sodium isovalerate mixed solution subjected to reaction in an oxidation device to an acidification kettle, and adding quantitative pure water; then, slowly adding sulfuric acid at a constant speed, releasing heat in the process, opening cooling circulating water, controlling the temperature of an acidification kettle below 100 ℃, gradually reducing the pH value of the material along with the reaction, and ending the acid addition when the pH value reaches a set value of pH 3.0; standing for a period of time to allow the isovaleric acid crude product and the sodium sulfate solution to be layered, finally discharging the sodium sulfate solution to a wastewater treatment tank, and discharging the crude isovaleric acid to an intermediate storage tank;
(3) rectification step
Firstly, conveying crude isovaleric acid in an intermediate storage tank into the rectifying tower through a pump, and introducing steam of 0.5-0.8 MPa (gauge pressure) into a reboiler at the bottom of the tower for heating; in the rectifying tower, because the boiling point of water is low, the water is continuously enriched in a gas phase and rises to the tower top, and the boiling point of isovaleric acid is high, the isovaleric acid is continuously enriched in a liquid phase and falls to the tower bottom, and the isovaleric acid is extracted to an isovaleric acid storage tank through a liquid phase outlet at the tower bottom.
2. The process and the device for producing the isovaleric acid by the isoamyl alcohol according to claim 1, wherein: the white oil with high selectivity is used as a reaction solvent, so that a reaction system can be quickly heated to 240 ℃, and the white oil has an emulsifying effect at high temperature, so that the melting speed of caustic soda and the dehydrogenation reaction speed of isoamyl alcohol are increased.
3. White oil is used as a solvent, and the reaction materials are in a liquid flow state in a cooling state, so that the defect that solid salt is not easy to unload in the cooling process in the solvent-free reaction is avoided, and the requirement on reaction equipment is lowered.
4. The process and the device for producing the isovaleric acid by the isoamyl alcohol according to claim 1, wherein: the temperature control is carried out through the heat conduction oil, so that the whole course of the oxidation process is at the optimal reaction temperature, and the nitrogen input, the hydrogen discharge, the raw material and catalytic addition speed and the product discharge speed are automatically controlled, so that the safe environment and the fastest reaction are obtained, and the production efficiency and the product quality are greatly improved.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210487914.XA CN115093318A (en) | 2022-05-06 | 2022-05-06 | Process and device for producing isovaleric acid from isoamyl alcohol |
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| CN202210487914.XA CN115093318A (en) | 2022-05-06 | 2022-05-06 | Process and device for producing isovaleric acid from isoamyl alcohol |
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| CN202210487914.XA Pending CN115093318A (en) | 2022-05-06 | 2022-05-06 | Process and device for producing isovaleric acid from isoamyl alcohol |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125810A (en) * | 2007-09-26 | 2008-02-20 | 河南庆安化工高科技股份有限公司 | Method for preparing isooctanoic acid |
| CN106748746A (en) * | 2017-02-23 | 2017-05-31 | 江西金泰化工股份有限公司 | A kind of isooctyl acid production system |
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2022
- 2022-05-06 CN CN202210487914.XA patent/CN115093318A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125810A (en) * | 2007-09-26 | 2008-02-20 | 河南庆安化工高科技股份有限公司 | Method for preparing isooctanoic acid |
| CN106748746A (en) * | 2017-02-23 | 2017-05-31 | 江西金泰化工股份有限公司 | A kind of isooctyl acid production system |
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