CN110981687A - Method for producing dichloroalkane compound and production device thereof - Google Patents
Method for producing dichloroalkane compound and production device thereof Download PDFInfo
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Abstract
The present invention relates to a method for producing a dichloroalkane compound and a production apparatus therefor, comprising: the preparation method comprises the steps of taking glycol, concentrated hydrochloric acid and hydrogen chloride gas as raw materials, carrying out continuous multi-stage chlorination reaction, continuous layering process and continuous washing process to obtain an organic phase, and carrying out rectification process to obtain the dichloroalkane compound. The invention adopts the continuous process to prepare the dichloroalkane compound, thereby reducing the production cost, reducing the labor intensity of operators, improving the labor efficiency, having stable production quality of products and achieving safe and environment-friendly production; the method of mixing hydrogen chloride gas and concentrated hydrochloric acid is adopted in the reaction process, no weak acid is generated, the reaction rate is increased, and the production efficiency is improved.
Description
Technical Field
The invention relates to a method for producing dichloroalkane compounds and a production device thereof, belonging to the technical field of chemical industry.
Background
The common dichloroalkanes in the market mainly comprise dichloropropane, dichlorobutane, dichloropentane, dichlorohexane and the like, are important fine chemical products, and can be used as medical intermediates, solvents and the like. The method for synthesizing dichloralkane includes thionyl chloride chlorination method, phosphorus oxychloride or phosphorus pentachloride chlorination method, hydrogen chloride gas catalytic chlorination method, concentrated hydrochloric acid catalytic chlorination method, etc.
The production of some halogenated hydrocarbons directly uses halogen to carry out halogenation reaction, the halogenation reaction also produces by-product hydrogen halide besides halogenated hydrocarbon, such as chlorination of alkane and aromatic hydrocarbon, and produces by-product hydrogen chloride gas, and some halogenation reactions, such as replacement reaction of hydrogen halide and halogenated hydrocarbon, and also produces by-product hydrogen halide, such as reaction of chlorinated hydrocarbon and hydrogen fluoride, and produces by-product hydrogen chloride while producing fluorohydrocarbon, and the hydrogen chloride gas by-product is low in price, so that the production of dichloroalkane by using hydrogen chloride or concentrated hydrochloric acid as raw material has the advantages of low raw material price and low cost.
Tetrahedron, vol.58, #36 P.7327-7334; journal of the chemical Society, Perkin Transactions 1: organic and Bio-Organic Chemistry (1972-1999, P.1855-1860) discloses a "tetrahydrofuran and concentrated hydrochloric acid process", wherein tetrahydrofuran and concentrated hydrochloric acid are reacted at high temperature and high pressure to obtain a product yield of about 78%, the main byproducts are chlorobutanol and chlorobutyl ether, the process has long time consumption, high energy consumption and higher requirements for equipment parameters, and the used raw material tetrahydrofuran is easy to generate peroxide and has certain potential safety risk.
Chinese patent document CN110330405A discloses a production process of 1, 4-dichlorobutane, which takes DMF as a catalyst, 1, 4-butanediol and triphosgene as reaction raw materials, reacts at 40-70 ℃, and collects yellowish oily liquid to finish the preparation of the 1, 4-dichlorobutane. The production process of the 1, 4-dichlorobutane is simple and convenient to operate, mild in reaction conditions, green, pollution-free, low-carbon and environment-friendly, and can realize large-scale production. However, 1, 4-butanediol and triphosgene are used as reaction raw materials, so that the production cost is high and the raw materials have high toxicity.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for producing a dichloroalkane compound and a production device thereof. The invention achieves the aim of safe and environment-friendly production through a continuous production process, the quality of the batch production product is stable, the light hydrochloric acid is not generated, the hydrochloric acid is recycled, and the circular economic production is realized.
The invention adopts the following technical scheme:
a process for producing a dichloroalkane compound comprising:
the preparation method comprises the steps of taking glycol, concentrated hydrochloric acid and hydrogen chloride gas as raw materials, carrying out continuous multi-stage chlorination reaction, continuous layering process and continuous washing process to obtain an organic phase, and carrying out rectification process to obtain the dichloroalkane compound.
According to the present invention, preferably, the diol has the following structure: OH-RO-H, R is C3-C10 alkyl. The dichloroalkane produced is represented by the following structural formula: Cl-R-Cl.
According to the invention, the mass concentration of the concentrated hydrochloric acid is preferably 30-35%.
According to the invention, the molar ratio of the diol, the concentrated hydrochloric acid and the hydrogen chloride gas is preferably 1 (1-3) to 1-3.
According to the invention, preferably, the reaction temperature of the multistage chlorination reaction is controlled to be 100-130 ℃, and the reaction pressure is controlled to be 0.2-0.5 MPa;
preferably, the multistage chlorination reaction is divided into 2-5 stages of chlorination reactions, and a plurality of reaction kettles are connected in series.
According to the present invention, it is preferable that the continuous layering step is a step of continuously layering the reaction solution obtained by the multistage chlorination reaction to separate an aqueous phase and an organic phase;
preferably, this is done by means of a stratified column.
According to the present invention, it is preferred that the organic phase obtained in the continuous layering step is subjected to a continuous washing step using an alkaline solution as a detergent, preferably a sodium carbonate solution. The mass concentration of the detergent is 5-10%, and the washing temperature is 30-50 ℃.
According to the present invention, preferably, the organic phase and the aqueous phase are obtained in the continuous washing step, the aqueous phase is recycled as a washing agent, and the organic phase is subjected to the rectification step to obtain the target dichloroalkane compound.
According to the present invention, it is preferred that the continuous washing process is carried out by a washing column. The washing tower is conventional equipment in the chemical field.
The invention also provides a device for producing dichloroalkane compounds, which comprises a multistage chlorination reaction system formed by connecting more than two chlorination reaction kettles in series, wherein the multistage chlorination reaction system is connected with the layering tower through a first material transferring pump, the bottom end of the layering tower is connected with the top end of the washing tower through a second material transferring pump, and the lower part of the washing tower is connected with a rectification system through a third material transferring pump.
According to the invention, preferably, the multistage chlorination reaction system comprises 2-5 chlorination reaction kettles which are connected in series.
According to the invention, preferably, a hydrogen chloride gas feeding hole and glycol and concentrated hydrochloric acid feeding holes are arranged at the top end of the chlorination reaction kettle;
preferably, the chlorination reaction kettle is provided with a stirring device and a heat-preservation interlayer.
According to the invention, preferably, the layered tower comprises a layered tower body, the layered tower body is of a cylindrical structure, and baffle plates are uniformly arranged in the middle of the layered tower body. Namely: the middle part of the layered tower body is provided with a baffle plate, and the upper part and the lower part of the layered tower body are hollow cylindrical bodies. The middle part of the layering tower is provided with a feed inlet, the reaction discharge of the chlorination reaction kettle is fed from the middle part of the layering tower, the materials are layered in the layering tower, the upper layer is a water phase, the materials are discharged from the top of the layering tower, and the organic phase is discharged from the bottom of the layering tower.
According to the invention, the top end of the layering tower is preferably connected with a hydrochloric acid recovery tank. Namely: after the layering by the layering tower, the organic phase enters the washing tower from the bottom end of the layering tower, and the aqueous phase enters the hydrochloric acid recovery tank from the top end of the layering tower.
According to the present invention, it is preferable that the bottom of the washing tower is connected to a reservoir for the alkaline liquid. Namely: the washing agent enters through the bottom end of the washing tower, is discharged from the top end of the washing tower after washing materials, and can enter the alkaline liquid storage tank for recycling.
According to the present invention, a process for producing a dichloroalkane compound, a preferred embodiment, comprises the steps of:
the method comprises a continuous multistage chlorination reaction process, a continuous layering process and a continuous washing process;
(1) a continuous multi-stage chlorination reaction process: continuously feeding glycol, concentrated hydrochloric acid and hydrogen chloride gas into a first-stage chlorination reaction kettle according to the molar ratio of 1 (1-3) to (1-3), and sequentially adding the mixture into other multi-stage chlorination reaction kettles, wherein the reaction temperature is controlled to be 100-130 ℃, and the reaction pressure is controlled to be 0.2-0.5 MPa to perform chlorination reaction, so as to obtain a reaction liquid I, namely a dichloroalkane mixture containing a small amount of weak hydrochloric acid;
(2) a continuous layering process: continuously feeding the reaction solution I into a layering tower, carrying out layering, feeding a water phase into a hydrochloric acid recovery tank, and feeding an organic phase II into a washing process;
(3) a continuous washing process: mixing, washing and layering an organic phase II and a 5-10% sodium carbonate solution in a washing tower at the temperature of 30-50 ℃ according to the mass ratio of 1 (2-5) to obtain an organic phase III and a water phase, feeding the water phase into a sodium carbonate storage tank for recycling, and rectifying the organic phase III to obtain a target product.
According to the production device for producing the dichloroalkane compound, raw materials are reacted through the continuous multi-stage chlorination reaction kettle, are continuously layered through the layering tower, are continuously washed through the washing tower, and the material conveying condition is performed through a high potential difference or a material transfer pump.
The reaction formula involved in the invention is as follows:
OH-R-OH+2HCl＝Cl-R-Cl+2H2O
the invention has not been described in detail, but is in accordance with the state of the art.
The invention has the following beneficial effects:
1. the invention adopts the continuous process to prepare the dichloroalkane compound, thereby reducing the production cost, reducing the labor intensity of operators, improving the labor efficiency, having stable production quality of products and achieving safe and environment-friendly production;
2. in the reaction process, a method of mixing hydrogen chloride gas and concentrated hydrochloric acid is adopted, and the hydrogen chloride gas is introduced to keep the concentration of the hydrochloric acid at more than 30 percent, so that weak acid is not generated, the reaction rate is improved, and the production efficiency is improved;
3. the invention adopts tower type liquid-liquid washing and separating equipment, effectively improves the reaction rate, accelerates the production process, and improves the production capacity and the device efficiency.
Drawings
FIG. 1 is a schematic view of the main structure of an apparatus for producing a dichloroalkane compound according to the present invention.
FIG. 2 is a schematic view showing the main structure of a layering tower in the apparatus for producing a dichloroalkane compound according to the present invention.
FIG. 3 is a gas chromatogram of 1, 4-dichlorobutane obtained in example 3 of the present invention.
FIG. 4 is a gas chromatogram of 1, 6-dichlorohexane obtained in example 5 of the present invention.
Wherein: 1. chlorination reaction kettle 2, first material transferring pump 3, layering tower 3-1, layering tower body 3-2, baffle plate 4, second material transferring pump 5, washing tower 6 and third material transferring pump.
Detailed Description
The present invention will be further described with reference to the following detailed description of embodiments thereof, but not limited thereto, in conjunction with the accompanying drawings.
The yields in the examples are molar yields.
Example 1
As shown in fig. 1 and 2, an apparatus for producing a dichloroalkane compound comprises a multistage chlorination reaction system composed of four chlorination reaction kettles 1 connected in series, the multistage chlorination reaction system is connected with a layering tower 3 through a first transfer pump 2, the bottom end of the layering tower 3 is connected with the top end of a washing tower 5 through a second transfer pump 4, and the lower part of the washing tower 5 is connected with a rectification system through a third transfer pump.
The top end of the chlorination reaction kettle 1 is provided with a hydrogen chloride gas feeding port and a glycol and concentrated hydrochloric acid feeding port; the chlorination reaction kettle 1 is provided with a stirring device and a heat-preservation interlayer.
The layered tower 3 comprises a layered tower body 3-1, the layered tower body 3-1 is of a cylindrical structure, and baffle plates 3-2 are uniformly arranged in the middle of the layered tower body 3-1. Namely: the middle part of the layered tower body 3-1 is provided with a baffle plate 3-2, and the upper part and the lower part are hollow cylindrical bodies. The middle part of the layering tower 3 is provided with a feed inlet, namely: the reaction discharge material of the chlorination reaction kettle 1 is fed from the middle part of the layering tower 3, the material is layered in the layering tower 3, the upper layer is a water phase, the material is discharged from the top of the layering tower 3, and the organic phase is discharged from the bottom of the layering tower 3.
The top end of the layering tower 3 is connected with a hydrochloric acid recovery tank. Namely: after being layered by the layering tower 3, the organic phase enters the washing tower 5 from the bottom end of the layering tower 3, and the aqueous phase enters the hydrochloric acid recovery tank from the top end of the layering tower 3.
The bottom end of the washing tower 5 is connected with a sodium carbonate storage tank. Namely: the sodium carbonate solution enters from the bottom end of the washing tower 5, is discharged from the top end of the washing tower 5 after being washed, and enters into the sodium carbonate solution storage tank for recycling.
Example 2
A process for producing a dichloroalkane compound comprising the steps of:
(1) a continuous multi-stage chlorination reaction process:
200kg/h of 1, 3-propylene glycol, 150kg/h of 33% concentrated hydrochloric acid and 150L/h of hydrogen chloride gas are continuously added into the first-stage chlorination reaction kettle 1 to carry out chlorination reaction, and reaction materials are transferred through the bottom of the kettle and sequentially enter other reaction kettles to carry out continuous heat preservation reaction. The pressure of the reaction system is 0.4MPa, the temperature of the first-stage reaction kettle is 105 ℃, the reaction temperature in other reaction kettles is 120 ℃, and the material in each reaction kettle stays for 2 hours to obtain reaction liquid I.
(2) A continuous layering process:
continuously feeding the reaction solution I into a layering tower 3, allowing a water phase to enter a hydrochloric acid recovery tank through layering, and allowing a brown yellow organic phase II to enter a washing process;
(3) a continuous washing process:
mixing, washing and layering an organic phase II and a 7% sodium carbonate solution in a washing tower 5 at the temperature of 30 ℃ according to the mass ratio of 1:3, feeding a water phase into a sodium carbonate storage tank for recycling, and rectifying an organic phase III to obtain a target product 1, 3-dichloropropane, wherein the purity is 99.63% by GC detection. The yield of the target product is 97.6%.
Example 3
A process for producing a dichloroalkane compound comprising the steps of:
(1) a continuous multi-stage chlorination reaction process:
200kg/h of 1, 4-butanediol, 120kg/h of 33% concentrated hydrochloric acid and 130L/h of hydrogen chloride gas are continuously added into a first-stage chlorination reaction kettle 1 for chlorination reaction, and reaction materials are transferred through the bottom difference of the kettle and sequentially enter other reaction kettles for continuous heat preservation reaction. The pressure of the reaction system is 0.4MPa, the temperature of the first-stage reaction kettle is 105 ℃, the reaction temperature in other reaction kettles is 120 ℃, and the material in each reaction kettle stays for 2 hours to obtain reaction liquid I.
(2) A continuous layering process:
continuously feeding the reaction solution I into a layering tower 3, allowing a water phase to enter a hydrochloric acid recovery tank through layering, and allowing a brown yellow organic phase II to enter a washing process;
(3) a continuous washing process:
mixing, washing and layering an organic phase II and an 8% sodium carbonate solution in a washing tower 5 at the temperature of 30 ℃ according to the mass ratio of 1:4, feeding a water phase into a sodium carbonate storage tank for recycling, and rectifying an organic phase III to obtain a target product 1, 4-dichlorobutane, wherein the purity is 99.87% by GC detection. The yield of the target product is 98%.
The gas chromatogram of 1, 4-dichlorobutane obtained in this example is shown in FIG. 3.
The gas chromatography data are as follows:
example 4
A process for producing a dichloroalkane compound comprising the steps of:
(1) a continuous multi-stage chlorination reaction process:
200kg/h of 1, 5-pentanediol, 110kg/h of 33% concentrated hydrochloric acid and 105L/h of hydrogen chloride gas are continuously added into a first-stage chlorination reaction kettle 1 to carry out chlorination reaction, and reaction materials are transferred through the bottom of the kettle and sequentially enter other reaction kettles to carry out continuous heat preservation reaction. The pressure of the reaction system is 0.35MPa, the temperature of the first-stage reaction kettle is 110 ℃, the reaction temperature in other reaction kettles is 125 ℃, and the material in each reaction kettle stays for 2 hours to obtain reaction liquid I.
(2) A continuous layering process:
continuously feeding the reaction solution I into a layering tower 3, layering, feeding a water phase into a hydrochloric acid recovery tank, and feeding a brown organic phase II into a washing process;
(3) a continuous washing process:
mixing, washing and layering an organic phase II and a 7% sodium carbonate solution in a washing tower 5 at the temperature of 30 ℃ according to the mass ratio of 1:2, feeding a water phase into a sodium carbonate storage tank for recycling, and rectifying an organic phase III to obtain a target product 1, 5-dichloropentane, wherein the purity is 99.52% by GC detection. The yield of the target product was 97.4%.
Example 5
A process for producing a dichloroalkane compound comprising the steps of:
(1) a continuous multi-stage chlorination reaction process:
200kg/h of 1, 6-hexanediol, 90kg/h of 33% concentrated hydrochloric acid and 100L/h of hydrogen chloride gas are continuously added into a first-stage chlorination reaction kettle 1 to carry out chlorination reaction, and reaction materials are transferred through the bottom of the kettle and sequentially enter other reaction kettles to carry out continuous heat preservation reaction. The pressure of the reaction system is 0.33MPa, the temperature of the first-stage reaction kettle is 110 ℃, the reaction temperature in other reaction kettles is 120 ℃, and the material in each reaction kettle stays for 2 hours to obtain reaction liquid I.
(2) A continuous layering process:
continuously feeding the reaction solution I into a layering tower 3, layering, feeding a water phase into a hydrochloric acid recovery tank, and feeding a brown organic phase II into a washing process;
(3) a continuous washing process:
mixing and washing the organic phase II and a 10% sodium carbonate solution in a washing tower 5 at a temperature of 30 ℃ according to a mass ratio of 1:2.5, layering, enabling the water phase to enter a sodium carbonate storage tank for recycling, and rectifying the organic phase III to obtain a target product 1, 6-dichlorohexane with a purity of 99.78% by GC detection. The yield of the target product is 97.8%.
The gas chromatogram of 1, 6-dichlorohexane obtained in this example is shown in FIG. 4.
The gas chromatography data are as follows:
example 6
A process for producing a dichloroalkane compound comprising the steps of:
(1) a continuous multi-stage chlorination reaction process:
200kg/h of 1, 7-heptanediol, 75kg/h of 33 percent concentrated hydrochloric acid and 85L/h of hydrogen chloride gas are continuously added into the first-stage chlorination reaction kettle 1 for chlorination reaction, and reaction materials are transferred through the bottom of the kettle and sequentially enter other reaction kettles for continuous heat preservation reaction. The pressure of the reaction system is 0.34MPa, the temperature of the first-stage reaction kettle is 110 ℃, the reaction temperature in other reaction kettles is 123 ℃, and the material in each reaction kettle stays for 2 hours to obtain reaction liquid I.
(2) A continuous layering process:
continuously feeding the reaction solution I into a layering tower 3, layering, feeding a water phase into a hydrochloric acid recovery tank, and feeding a brown organic phase II into a washing process;
(3) a continuous washing process:
mixing, washing and layering the organic phase II and a 7% sodium carbonate solution in a washing tower 5 at the temperature of 30 ℃ according to the mass ratio of 1:2.5, feeding the water phase into a sodium carbonate storage tank for recycling, and rectifying the organic phase III to obtain a target product 1, 7-dichloroheptane, wherein the purity is 99.46% by GC detection. The yield of the target product was 97.3%.
Comparative example 1
200kg of 1, 6-hexanediol and 1400kg of 33% concentrated hydrochloric acid are continuously added into a chlorination reaction kettle, the reaction is carried out for 8 hours under the pressure of 0.33MPa, after the reaction is finished, an upper aqueous phase is transferred to a hydrochloric acid recovery tank, a lower organic phase is transferred to an alkaline washing kettle for washing, after the alkaline washing is finished, the organic phase is rectified and purified through a rectification process to obtain a target product 1, 6-dichlorohexane, and the purity is 99.5% through GC detection. The yield of the target product is 92%.
It can be seen that the chlorination reaction proceeds only in the first stage, and as the concentration of the starting material decreases in the latter stage, the yield of the product decreases without increasing the concentration of hydrochloric acid. The addition of concentrated hydrochloric acid is much higher than that of hydrogen chloride gas. Therefore, the method simultaneously uses concentrated hydrochloric acid and hydrogen chloride gas, and improves the reaction yield to a great extent through multi-stage chlorination reaction, layering and continuous washing.
Claims (10)
1. A process for producing a dichloroalkane compound comprising:
the preparation method comprises the steps of taking glycol, concentrated hydrochloric acid and hydrogen chloride gas as raw materials, carrying out continuous multi-stage chlorination reaction, continuous layering process and continuous washing process to obtain an organic phase, and carrying out rectification process to obtain the dichloroalkane compound.
2. The process for producing a dichloroalkane compound according to claim 1, wherein the diol has the following structure: OH-RO-H, R is C3-C10 alkyl.
3. The process for producing a dichloroalkane compound according to claim 1, wherein the concentrated hydrochloric acid is at a concentration of 30 to 35% by mass.
4. The method for producing a dichloroalkane compound according to claim 1, wherein the molar ratio of the diol, the concentrated hydrochloric acid and the hydrogen chloride gas is 1 (1-3) to (1-3).
5. The method for producing a dichloroalkane compound according to claim 1, wherein the reaction temperature of the multistage chlorination reaction is controlled to 100 to 130 ℃, and the reaction pressure is controlled to 0.2 to 0.5 MPa;
preferably, the multistage chlorination reaction is divided into 2-5 stages of chlorination reactions, and a plurality of reaction kettles are connected in series.
6. The process for producing a dichloroalkane compound according to claim 1, wherein the continuous layering step comprises continuously layering a reaction solution obtained by the multistage chlorination reaction to separate an aqueous phase and an organic phase;
carrying out a continuous washing procedure on the organic phase obtained in the continuous layering procedure, wherein the detergent used in the continuous washing procedure is an alkaline solution;
preferably, the organic phase and the aqueous phase are obtained in the continuous washing process, the aqueous phase is recycled as a washing agent, and the target product dichloroalkane compound is obtained from the organic phase through the rectification process.
7. The device for producing the dichloroalkane compound comprises a multistage chlorination reaction system formed by connecting more than two chlorination reaction kettles in series, wherein the multistage chlorination reaction system is connected with a layering tower through a first material transferring pump, the bottom end of the layering tower is connected with the top end of a washing tower through a second material transferring pump, and the lower part of the washing tower is connected with a rectification system through a third material transferring pump.
8. The apparatus for producing a dichloroalkane compound according to claim 7, wherein said multistage chlorination reaction system comprises 2 to 5 chlorination reactors connected in series.
9. The apparatus for producing a dichloroalkane compound according to claim 7, wherein the stratified column comprises a stratified column body having a cylindrical structure, and baffles are uniformly arranged in the middle of the stratified column body.
10. The apparatus for producing a dichloroalkane compound according to claim 7, wherein the top end of the layering tower is connected to a hydrochloric acid recovery tank, and the bottom end of the washing tower is connected to a basic liquid storage tank.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112341309A (en) * | 2020-11-30 | 2021-02-09 | 山东嘉成医药科技有限公司 | Preparation method of dichloroalkane |
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Application publication date: 20200410 |