CN114573633A - Preparation process of triisopropyl phosphate - Google Patents
Preparation process of triisopropyl phosphate Download PDFInfo
- Publication number
- CN114573633A CN114573633A CN202210166432.4A CN202210166432A CN114573633A CN 114573633 A CN114573633 A CN 114573633A CN 202210166432 A CN202210166432 A CN 202210166432A CN 114573633 A CN114573633 A CN 114573633A
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- China
- Prior art keywords
- sealing cover
- reaction kettle
- triisopropyl phosphate
- cyclohexane
- cooling
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/11—Esters of phosphoric acids with hydroxyalkyl compounds without further substituents on alkyl
Abstract
The invention discloses a preparation process of triisopropyl phosphate, which relates to the field of synthesis of triisopropyl phosphate and comprises a reaction kettle and a cooling mechanism, wherein a sealing cover is arranged at the upper end of the reaction kettle, a feeding pipe is arranged at the position, close to one side, of the upper end of the sealing cover, a sealing valve is arranged between the inner side walls of the feeding pipe and close to the top, an insertion pipe is arranged at the position, close to the other side, of the upper end of the sealing cover, a thermometer is movably inserted in the insertion pipe, a sealing gasket is arranged at the upper end of the sealing cover and close to the middle, a stirring mechanism is arranged on the sealing cover, and the stirring mechanism comprises a supporting plate; according to the invention, the reaction kettle can be cooled in a water bath mode, the temperature regulation is convenient and fast, the temperature change is stable, the position of the bottom of the stirring shaft can be adjusted by a worker according to the amount of the liquid medicine, the liquid medicine is convenient to stir, and the stirring effect is better.
Description
Technical Field
The invention relates to the field of synthesis of triisopropyl phosphate, in particular to a preparation process of triisopropyl phosphate.
Background
Phosphate esters, also known as orthophosphate (to distinguish them from phosphites), are ester derivatives of phosphoric acid and belong to the class of phosphoric acid derivatives. The phosphate ester is mainly used as phosphorus-containing pesticide, nerve gas, fire-retardant hydraulic oil, lubricating oil and the like.
Triisopropyl phosphate is a halogen-free phosphate flame-retardant plasticizer, and does not pollute the environment twice; the phosphate variety belongs to the model with the lowest viscosity and the highest phosphorus content. The product is colorless and transparent, has good intermiscibility, can retard flame and plasticize, plays a balance role between a flame retardant and a plasticizing material, and can ensure that the processed material does not change the natural color and the physical property of the processed material.
Most of common preparation processes of triisopropyl phosphate in the market are inconvenient to adjust the temperature inside a reaction kettle, the temperature change is fast, liquid medicine inside the reaction kettle is inconvenient to stir, and the stirring effect is poor, so that the preparation process of triisopropyl phosphate is provided.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a preparation process of triisopropyl phosphate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation process of triisopropyl phosphate comprises the following steps:
step S001: putting cyclohexane into a reaction kettle, cooling by a cooling mechanism, and pumping phosphorus trichloride at a controlled temperature of 0-5 ℃ to prepare a phosphorus trichloride cyclohexane mixed solution;
step S002: putting cyclohexane, isopropanol and triethylamine into a reaction kettle, cooling to 0-5 ℃, and dropwise adding a phosphorus trichloride cyclohexane mixed solution; keeping the temperature at 0-5 ℃ and reacting for 6-8 hours;
step S003: adding water for hydrolysis, washing with 5% sodium carbonate aqueous solution once, washing with water twice, dehydrating anhydrous sodium sulphate, and evaporating out cyclohexane solvent to obtain crude product;
step S004: and (4) carrying out high vacuum rectification on the crude product, collecting positive-boiling residues, and carrying out mixed batch packaging after the positive-boiling residues are analyzed to be qualified to obtain a finished product.
Further, in the step S001, the charging weight ratio of cyclohexane to phosphorus trichloride is as follows: (7-7.1): 1; in the step S002, the charging weight ratio of cyclohexane, isopropanol and triethylamine is as follows: (5.2-5.4): 1: (1.8-1.9).
Further, a sealing cover is arranged at the upper end of the reaction kettle, a feeding pipe is arranged at the upper end of the sealing cover close to one side, a sealing valve is arranged between the inner side walls of the feeding pipe close to the top, an insertion pipe is arranged at the upper end of the sealing cover close to the other side, a thermometer is movably inserted in the insertion pipe, a sealing gasket is arranged at the upper end of the sealing cover close to the middle, and a stirring mechanism is arranged on the sealing cover.
Further, rabbling mechanism includes the backup pad, the activity groove has been seted up to the backup pad upper end, the activity inslot lateral wall is close to top position and has seted up the recess, be provided with the gear between the recess inside wall, the activity of activity inslot portion is provided with the extension board, the extension board is close to gear one side equidistance and has seted up a plurality of groups tooth's socket, and is two sets of run through between the backup pad and be provided with the pivot, the equal threaded connection in pivot both ends is provided with fixation nut, four groups the extension board upper end is provided with the loading board, the loading board upper end is provided with the motor, the loading board bottom is close to the intermediate position and is provided with the (mixing) shaft.
Further, the extension board passes through tooth's socket cooperation gear setting inside the activity inslot, pivot one end is passed the recess inside wall and is run through the gear setting, (mixing) shaft one end is passed sealed the pad and is set up inside reation kettle with sealed lid activity, the output shaft fixed connection of loading board and motor is passed at the (mixing) shaft top.
Furthermore, the cooling mechanism comprises a cooling box, a heat insulation pad is arranged on the outer side wall of the cooling box, a cavity is formed in the side wall of the cooling box, and an air tank and a liquid nitrogen tank are arranged on one side of the cooling box.
Further, the air tank and the liquid nitrogen tank are connected with the cavity through air pipes, water is filled in the cooling box, and a pressure release valve communicated with the cavity is arranged at the top of the cooling box.
Further, the bottom of the insertion pipe and the bottom of the feeding pipe penetrate through the sealing cover and are movably arranged inside the reaction kettle, and the sealing cover is in threaded connection with the reaction kettle.
Compared with the prior art, the invention has the beneficial effects that:
1. place reation kettle inside the cooler bin, and add water to the cooler bin is inside, add the liquid nitrogen to the cavity is inside through liquid nitrogen container and trachea, can absorb the heat during liquid nitrogen gasification and make cooler bin lateral wall temperature reduce, and then make the temperature descend, the lower water of temperature can make its inside ethylene ring temperature reduce to reation kettle cooling, observe the inside temperature variation of reation kettle through the thermometer, when the temperature is lower, stop adding the liquid nitrogen and open the relief valve, let in inside the cavity with the inside air of air tank, thereby discharge the inside nitrogen gas concentration of diluting nitrogen gas of cavity, make the temperature slowly rise, wherein the heat preservation pad can play fine heat preservation effect and avoid the temperature to scatter and disappear, the staff of being convenient for adjusts the inside temperature of reation kettle, and temperature variation is comparatively stable.
2. Make the inside gear rotation of recess through the pivot, the extension board passes through the tooth's socket and removes to the activity inslot portion gradually this moment to making the loading board to moving near backup pad position, driving the (mixing) shaft bottom and removing to the middle part position of the inside liquid medicine of reation kettle, later making the (mixing) shaft rotatory through the motor stir the liquid medicine, the staff can be convenient for stir the liquid medicine according to the position of the volume adjustment (mixing) shaft bottom of liquid medicine, and stirring effect is better.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
FIG. 1 is a schematic diagram of the overall structure of a process for preparing triisopropyl phosphate according to the present invention;
FIG. 2 is a schematic structural diagram of a sealing cover and a stirring mechanism of a preparation process of triisopropyl phosphate provided by the invention;
FIG. 3 is an enlarged view of the point A in FIG. 2 of the process for preparing triisopropyl phosphate according to the present invention;
FIG. 4 is a schematic structural view of a cooling tank of a process for producing triisopropyl phosphate according to the present invention;
FIG. 5 is a flow chart of a process for preparing triisopropyl phosphate according to the present invention.
In the figure: 1. a reaction kettle; 2. a sealing cover; 3. a feed tube; 4. a sealing valve; 5. inserting a tube; 6. a thermometer; 7. a gasket; 8. a stirring mechanism; 9. a support plate; 10. a movable groove; 11. a groove; 12. a gear; 13. a rotating shaft; 14. fixing a nut; 15. a support plate; 16. a tooth socket; 17. a motor; 18. a stirring shaft; 19. a cooling mechanism; 20. a cooling tank; 21. a heat-insulating pad; 22. a cavity; 23. an air tank; 24. a liquid nitrogen tank; 25. a carrier plate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "end", "near", "side", "top", "middle", "bottom", "inner", "outer", and the like, indicate orientations and positional relationships based on the orientations and positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
Example 1
Referring to fig. 1 and 4, the present invention provides a technical solution: the preparation process of the triisopropyl phosphate comprises a reaction kettle 1 and a cooling mechanism 19, wherein a sealing cover 2 is arranged at the upper end of the reaction kettle 1, a feeding pipe 3 is arranged at the position, close to one side, of the upper end of the sealing cover 2, a sealing valve 4 is arranged between the inner side walls of the feeding pipe 3 and close to the top, an insertion pipe 5 is arranged at the position, close to the other side, of the upper end of the sealing cover 2, a thermometer 6 is movably inserted into the insertion pipe 5, a sealing gasket 7 is arranged at the position, close to the middle, of the upper end of the sealing cover 2, and a stirring mechanism 8 is arranged on the sealing cover 2.
Referring to fig. 4, the cooling mechanism 19 includes a cooling box 20, a thermal pad 21 is disposed on an outer side wall of the cooling box 20, a cavity 22 is formed in a side wall of the cooling box 20, and an air tank 23 and a liquid nitrogen tank 24 are disposed on one side of the cooling box 20.
As an embodiment provided by the present invention, preferably, the air tank 23 and the liquid nitrogen tank 24 are both connected to the cavity 22 through an air pipe, the cooling box 20 is filled with water, and the top of the cooling box 20 is provided with a pressure release valve communicated with the cavity 22; the bottom of the cannula 5 and the bottom of the charging pipe 3 are both movably arranged inside the reaction kettle 1 through the sealing cover 2, and the sealing cover 2 is in threaded connection with the reaction kettle 1.
When in use, a worker adds cyclohexane into a reaction kettle 1, then installs a sealing cover 2 provided with a stirring mechanism 8 at the top of the reaction kettle 1, passes one end of a thermometer 6 through an insertion tube 5 and is arranged inside the reaction kettle 1, then places the reaction kettle 1 inside a cooling box 20, adds water into the cooling box 20, adds liquid nitrogen into a cavity 22 through a liquid nitrogen tank 24 and an air pipe, absorbs heat during gasification of the liquid nitrogen to reduce the temperature of the side wall of the cooling box 20 and further reduce the water temperature, cools the reaction kettle 1 by the water with lower temperature to reduce the temperature of ethylene ring inside the reaction kettle 1, observes the temperature change inside the reaction kettle 1 through the thermometer 6, stops adding the liquid nitrogen and opens a pressure release valve when the temperature is lower, introduces air inside an air tank 23 into the cavity 22, discharges the nitrogen inside the cavity 22 to dilute the concentration of the nitrogen, and slowly raises the water temperature, when the temperature in the reaction kettle 1 is controlled within the range of 0-5 ℃, the addition of liquid nitrogen and air is stopped, wherein the heat insulation pad 21 can play a good heat insulation effect to avoid temperature loss.
Example 2
Referring to fig. 1-3, the present invention provides a technical solution: the utility model provides a preparation technology of triisopropyl phosphate, still include rabbling mechanism 8, rabbling mechanism 8 includes backup pad 9, movable groove 10 has been seted up to backup pad 9 upper end, movable groove 10 inside wall is close to top position and has seted up recess 11, be provided with gear 12 between the recess 11 inside wall, the inside activity of movable groove 10 is provided with extension board 15, extension board 15 is close to gear 12 one side equidistance and has seted up a plurality of groups tooth's socket 16, it is provided with pivot 13 to run through between two sets of backup pads 9, the equal threaded connection in pivot 13 both ends is provided with fixation nut 14, the 15 upper ends of four groups of extension boards are provided with loading board 25, loading board 25 upper end is provided with motor 17, loading board 25 bottom is close to the intermediate position and is provided with (mixing) shaft 18.
As an embodiment provided by the present invention, preferably, the support plate 15 is disposed inside the movable groove 10 by engaging the gear 12 through the tooth slot 16, one end of the rotating shaft 13 is disposed through the inner sidewall of the groove 11 and penetrates the gear 12, one end of the stirring shaft 18 is movably disposed inside the reaction vessel 1 by penetrating the sealing gasket 7 and the sealing cover 2, and the top of the stirring shaft 18 is fixedly connected to the output shaft of the motor 17 by penetrating the bearing plate 25.
Specifically, seal valve 4 is opened, slowly add phosphorus trichloride to reation kettle 1 through filling tube 3 inside, then make the inside gear 12 of recess 11 rotatory through pivot 13, support board 15 moves inside to movable groove 10 through tooth's socket 16 gradually this moment, thereby make loading board 25 to being close to backup pad 9 position removal, drive the middle part position that (mixing) shaft 18 bottom moved to the inside liquid medicine of reation kettle 1, later make the (mixing) shaft 18 rotatory through motor 17 stir the liquid medicine, wherein sealed pad 7 has the liquid medicine to ooze when can avoiding the (mixing) shaft 18 stirring, thereby make cyclohexane and income phosphorus trichloride intensive mixing, formulate the mixed liquid of phosphorus trichloride cyclohexane.
Example 3
As shown in fig. 5, a preparation process of triisopropyl phosphate comprises the following steps:
step S001: putting cyclohexane into a reaction kettle 1, cooling by a cooling mechanism 19, and slowly pumping phosphorus trichloride at a temperature of 0-5 ℃ to prepare phosphorus trichloride cyclohexane mixed solution;
step S002: adding cyclohexane, isopropanol and triethylamine into a reaction kettle 1, cooling to 0-5 ℃, and slowly dropwise adding a phosphorus trichloride cyclohexane mixed solution; keeping the temperature at 0-5 ℃ and reacting for 6-8 hours; the content of the middle sample is about 90 percent; the chemical reaction formula is as follows:
step S003: adding water for hydrolysis, washing once with 5% sodium carbonate aqueous solution, washing twice with water, dehydrating anhydrous sodium sulphate, and evaporating out cyclohexane solvent to obtain crude product content: 93-97 percent;
step S004: the crude product is refined and distilled in high vacuum, the normal boiling substance is collected, and after being analyzed to be qualified, the product is mixed and packaged to obtain the finished product, only the cyclohexane solvent is removed, other post-treatments are not needed, and the reaction kettle 1 is not corroded, so that the investment and the energy consumption of the reaction kettle 1 can be saved, and the operation is more convenient.
As an embodiment provided by the present invention, preferably, the charging weight of cyclohexane and phosphorus trichloride in step S001 is: 290g, 41 g; in the step S002, the charging weight ratio of cyclohexane, isopropanol and triethylamine is as follows: 320g, 60g and 111g, and the content of the prepared crude product is as follows: 96.1 percent.
As another embodiment provided by the present invention, preferably, the charging weight of cyclohexane and phosphorus trichloride in step S001 is: 318g and 45 g; in the step S002, the charging weight ratio of cyclohexane, isopropanol and triethylamine is as follows: 350g, 66g and 120g, and the content of the prepared crude product is as follows: 95 percent.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The preparation process of triisopropyl phosphate is characterized by comprising the following steps of:
step S001: putting cyclohexane into a reaction kettle (1), cooling by a cooling mechanism (19), and pumping phosphorus trichloride at a temperature of 0-5 ℃ to prepare phosphorus trichloride cyclohexane mixed solution;
step S002: putting cyclohexane, isopropanol and triethylamine into a reaction kettle (1), cooling to 0-5 ℃, and then dropwise adding a phosphorus trichloride cyclohexane mixed solution; keeping the temperature at 0-5 ℃ and reacting for 6-8 hours;
step S003: adding water for hydrolysis, washing with 5% sodium carbonate aqueous solution once, washing with water twice, dehydrating anhydrous sodium sulphate, and evaporating out cyclohexane solvent to obtain crude product;
step S004: and (4) performing high-vacuum rectification on the crude product, collecting positive-boiling residues, and performing mixed batch packaging after the positive-boiling residues are analyzed to be qualified to obtain a finished product.
2. The process for preparing triisopropyl phosphate according to claim 1, wherein the charging weight ratio of cyclohexane to phosphorus trichloride in step S001 is: (7-7.1): 1; in the step S002, the charging weight ratio of cyclohexane, isopropanol and triethylamine is as follows: (5.2-5.4): 1: (1.8-1.9).
3. The process for preparing triisopropyl phosphate according to claim 1, wherein an insertion tube (5) is arranged on the reaction kettle (1), a thermometer (6) is movably inserted in the insertion tube (5), a sealing gasket (7) is arranged at the upper end of a sealing cover (2) of the reaction kettle (1) close to the middle position, and a stirring mechanism (8) penetrating through the sealing cover (2) is arranged on the sealing cover.
4. The process for preparing triisopropyl phosphate as claimed in claim 3, wherein the stirring mechanism (8) comprises a supporting plate (9), a movable groove (10) is formed at the upper end of the supporting plate (9), a groove (11) is formed in the inner side wall of the movable groove (10) near the top, a gear (12) is arranged between the inner side walls of the grooves (11), supporting plates (15) are movably arranged in the movable groove (10), a rotating shaft (13) penetrates between two groups of the supporting plates (9), bearing plates (25) are arranged at the upper ends of four groups of the supporting plates (15), a motor (17) is arranged at the upper ends of the bearing plates (25), and a stirring shaft (18) is arranged at the bottom end of the bearing plates (25) near the middle position.
5. The preparation process of triisopropyl phosphate as claimed in claim 4, wherein a plurality of groups of tooth grooves (16) are equidistantly formed on one side of the support plate (15) close to the gear (12), and the support plate (15) is arranged inside the movable groove (10) through the tooth grooves (16) in cooperation with the gear (12).
6. The preparation process of triisopropyl phosphate as claimed in claim 4, wherein fixing nuts (14) are arranged at both ends of the rotating shaft (13) in a threaded connection manner, one end of the rotating shaft (13) penetrates through the inner side wall of the groove (11) and penetrates through the gear (12), one end of the stirring shaft (18) penetrates through the sealing gasket (7) and the sealing cover (2) and is movably arranged inside the reaction kettle (1), and the top of the stirring shaft (18) penetrates through the bearing plate (25) and is fixedly connected with the output shaft of the motor (17).
7. The process for preparing triisopropyl phosphate as claimed in claim 1, wherein the cooling mechanism (19) comprises a cooling tank (20), the outer side wall of the cooling tank (20) is provided with a heat insulating pad (21), the side wall of the cooling tank (20) is provided with a cavity (22), and one side of the cooling tank (20) is provided with an air tank (23) and a liquid nitrogen tank (24).
8. The preparation process of triisopropyl phosphate as claimed in claim 7, wherein the air tank (23) and the liquid nitrogen tank (24) are both connected with the cavity (22) through air pipes, water is filled in the cooling tank (20), and a pressure release valve communicated with the cavity (22) is arranged at the top of the cooling tank (20).
9. The process for preparing triisopropyl phosphate as claimed in claim 3, wherein a sealing cover (2) is disposed at the upper end of the reaction kettle (1), a feeding pipe (3) is disposed at the upper end of the sealing cover (2) near one side, a sealing valve (4) is disposed between the inner side walls of the feeding pipe (3) near the top, and a cannula (5) is disposed at the upper end of the sealing cover (2) near the other side.
10. The process for preparing triisopropyl phosphate as claimed in claim 9, wherein the bottom of the cannula (5) and the bottom of the feeding tube (3) are movably arranged inside the reaction kettle (1) through a sealing cover (2), and the sealing cover (2) is in threaded connection with the reaction kettle (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202210166432.4A CN114573633A (en) | 2022-02-23 | 2022-02-23 | Preparation process of triisopropyl phosphate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210166432.4A CN114573633A (en) | 2022-02-23 | 2022-02-23 | Preparation process of triisopropyl phosphate |
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| CN202210166432.4A Pending CN114573633A (en) | 2022-02-23 | 2022-02-23 | Preparation process of triisopropyl phosphate |
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Citations (6)
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| JP2004018815A (en) * | 2002-06-20 | 2004-01-22 | Daihachi Chemical Industry Co Ltd | Flame-retardant for polyurethane resin, premix composition for flame-retardant polyurethane foam, and manufacturing method of flame-retardant polyurethane foam |
| CN101250199A (en) * | 2008-03-20 | 2008-08-27 | 太仓市茜泾化工有限公司 | Method for preparing diisopropyl phosphite |
| CN211051497U (en) * | 2019-10-28 | 2020-07-21 | 常熟市金申医化制品有限责任公司 | Reation kettle is used in sulfadoxine production |
| CN212595710U (en) * | 2020-06-25 | 2021-02-26 | 上高金安实业有限公司 | Reation kettle that phosphorus trichloride was used |
| CN213376611U (en) * | 2020-09-05 | 2021-06-08 | 宁夏忠同生物科技有限公司 | Quick refrigerated ultra-low temperature reation kettle |
| CN215611566U (en) * | 2021-09-16 | 2022-01-25 | 洛阳市三诺化工有限公司 | Neutralization reaction kettle for preparing triisobutyl phosphate |
-
2022
- 2022-02-23 CN CN202210166432.4A patent/CN114573633A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2004018815A (en) * | 2002-06-20 | 2004-01-22 | Daihachi Chemical Industry Co Ltd | Flame-retardant for polyurethane resin, premix composition for flame-retardant polyurethane foam, and manufacturing method of flame-retardant polyurethane foam |
| CN101250199A (en) * | 2008-03-20 | 2008-08-27 | 太仓市茜泾化工有限公司 | Method for preparing diisopropyl phosphite |
| CN211051497U (en) * | 2019-10-28 | 2020-07-21 | 常熟市金申医化制品有限责任公司 | Reation kettle is used in sulfadoxine production |
| CN212595710U (en) * | 2020-06-25 | 2021-02-26 | 上高金安实业有限公司 | Reation kettle that phosphorus trichloride was used |
| CN213376611U (en) * | 2020-09-05 | 2021-06-08 | 宁夏忠同生物科技有限公司 | Quick refrigerated ultra-low temperature reation kettle |
| CN215611566U (en) * | 2021-09-16 | 2022-01-25 | 洛阳市三诺化工有限公司 | Neutralization reaction kettle for preparing triisobutyl phosphate |
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