CN216005719U - System device for continuously preparing trans-1, 3-dichloropropene - Google Patents
System device for continuously preparing trans-1, 3-dichloropropene Download PDFInfo
- Publication number
- CN216005719U CN216005719U CN202122451468.0U CN202122451468U CN216005719U CN 216005719 U CN216005719 U CN 216005719U CN 202122451468 U CN202122451468 U CN 202122451468U CN 216005719 U CN216005719 U CN 216005719U
- Authority
- CN
- China
- Prior art keywords
- dichloropropene
- reaction
- trans
- rectification
- unit
- 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 utility model provides a system device for continuously preparing trans-1, 3-dichloropropene, which comprises a first chlorination reaction unit, a first rectification unit, a second reaction unit and a second rectification unit which are connected in sequence; the second reaction unit comprises a catalytic reaction device and an extraction reaction device which are connected in sequence; and the top of the separation and purification tower in the second rectifying unit is connected with the inlet of the second reaction unit. The system device prepares 1, 3-dichloropropene through a first chlorination reaction unit, and then obtains trans-1, 3-dichloropropene and cis-1, 3-dichloropropene through rectification and separation of a first rectification unit, and the cis-1, 3-dichloropropene is subjected to secondary rectification and separation after catalytic reaction and extraction reaction to obtain the trans-1, 3-dichloropropene with high added value, so that the continuous preparation of the DD mixed agent to the trans-1, 3-dichloropropene is realized, and the economic effect is improved.
Description
Technical Field
The utility model relates to a chemical plant technical field especially relates to a system's device of serialization preparation trans-1, 3-dichloropropene.
Background
1, 3-dichloropropene has wide application in the fields of medicine and agriculture, and trans-1, 3-dichloropropene is mainly used for synthesizing chloroallyloxyamine (an intermediate of cyclohexenone herbicides) and synthesizing terbinafine hydrochloride which is an antifungal medicine. However, trans-1, 3-dichloropropene with the concentration of 95 percent is mainly used in the current market, and can only be applied to the production of pesticide intermediates. The medical field needs trans-1, 3-dichloropropene with purity of more than 99 percent, and the conventional one-step rectification is difficult to obtain the trans-1, 3-dichloropropene with purity of more than 99 percent, so the rectification mode needs to be improved so as to obtain the trans-1, 3-dichloropropene with purity of more than 99 percent.
The prior trans-1, 3-dichloropropene is mostly prepared by adopting a continuous rectification method, on one hand, a small amount of mixed dichloropropene existsBoiling point of dichloropropene being close to C6Impurities cause that 99 percent of trans-1, 3-dichloropropene is difficult to prepare, and on the other hand, a large amount of cis-1, 3-dichloropropene byproduct is only treated as solid waste, so that the utilization rate of raw materials for producing the trans-1, 3-dichloropropene by using the method is not high, and the economic benefit is low.
CN110498728A discloses a trans-1, 3-dichloropropene and cis-1, 3-dichloropropene compound and a process flow thereof, wherein the method adopts a four-tower continuous rectification process to prepare cis-form and trans-1, 3-dichloropropene after rectification and separation.
CN208471941U discloses a refining device of trans-1, 3-dichloropropene, in which a method for separating trans-1, 3-dichloropropene by extractive distillation is disclosed.
Therefore, the existing method for producing trans-1, 3-dichloropropene is mostly limited to rectification separation, and a method for producing trans-1, 3-dichloropropene by using cis-1, 3-dichloropropene has not been reported.
US3914167A discloses a method for isomerizing trans-1, 3-dichloropropene to cis-1, 3-dichloropropene, which synthesizes cis-1, 3-dichloropropene by a catalyst under the condition of ultraviolet light illumination, and CN109694308A discloses a method for synthesizing cis-1, 3-dichloropropene by in-situ transposition of trans-1, 3-dichloropropene, wherein a photo-promoter is added to synthesize cis-1, 3-dichloropropene by in-situ transposition under the condition of ultraviolet light illumination.
Although the prior art of synthesizing cis-1, 3-dichloropropene by using trans-1, 3-dichloropropene as a raw material lacks economic value for producing cis-1, 3-dichloropropene by using trans-1, 3-dichloropropene as a raw material under the current market conditions.
Aiming at the problem of low added value of the mixed dichloropropene crude product, a set of device and process capable of converting the mixed dichloropropene crude product into high-purity trans-1, 3-dichloropropene need to be developed, so that the added value of a chloropropene downstream product is greatly improved.
SUMMERY OF THE UTILITY MODEL
In view of the problems existing in the prior art, the utility model provides a system device for continuously preparing trans-1, 3-dichloropropene, the system device can realize that mixed dichloropropene crude product (DD mixes the agent) is continuous to the preparation of high-purity trans-1, 3-dichloropropene, has solved the problem that current mixed dichloropropene crude product added value is low.
To achieve the purpose, the utility model adopts the following technical proposal:
the utility model provides a system device for continuously preparing trans-1, 3-dichloropropene, which comprises a first chlorination reaction unit, a first rectification unit, a second reaction unit and a second rectification unit which are connected in sequence; the second reaction unit comprises a catalytic reaction device and an extraction reaction device which are connected in sequence; and the top of the separation and purification tower in the second rectifying unit is connected with the inlet of the second reaction unit.
System's device carries out chlorination through first chlorination unit, can mix the C in the agent with DD6And (2) converting the impurities into a chloropropene mixture, then entering a first rectification unit for carrying out first rectification to separate heavy component impurities and collecting a first part of trans-1, 3-dichloropropene products, carrying out transposition reaction on the cis-1, 3-dichloropropene obtained by separation by a catalytic reaction device of a second reaction unit to convert the cis-1, 3-dichloropropene into trans-1, 3-dichloropropene, then extracting by an extraction reaction device to remove a catalyst for reaction, sending the obtained mixed dichloropropene into a second rectification unit for rectification and separation, and collecting a second part of trans-1, 3-dichloropropene products.
The utility model discloses in the second rectification unit the top of the tower of separation and purification tower with the entry of second reaction unit links to each other, can carry the second reaction unit middle circulation reaction back to the cis-1, 3-dichloropropene that second reaction unit did not react completely, improved the utilization ratio of raw materials.
The system device can realize the DD mixes the agent to trans-1, 3-dichloropropene's serialization conversion, and economic benefits is showing and is strengthening.
The DD mixture contains 1, 2-dichloropropane, 3-dichloropropene, 3-chloro-1, 5-hexadiene, cis-1, 3-dichloropropene, trans-1, 3-dichloropropene, 6-chloro-1-hexene and the like.
The DD mixture comprises, by mass, 0.01-20% of 1, 2-dichloropropane, 0.5-2% of 3, 3-dichloropropene, 0.1-1.5% of 3-chloro-1, 5-hexadiene, 40-60% of cis-1, 3-dichloropropene, 35-55% of trans-1, 3-dichloropropene and 0.5-2.5% of 6-chloro-1-hexene.
Among them, 1, 2-dichloropropane may be 0.01 to 20%, for example, 0.01%, 0.05%, 0.08%, 0.1%, 0.12%, 0.15%, 0.2%, 1%, 5%, 10%, 15%, 20%, or the like.
The 3, 3-dichloropropene may be 0.5 to 2%, for example, 0.5%, 0.8%, 1.0%, 1.2%, 1.5%, or 2.0%.
The 3-chloro-1, 5-hexadiene content may be 0.1 to 1.5%, for example, 0.1%, 0.2%, 0.3%, 0.5%, 0.8%, 1.0%, 1.2%, or 1.5%.
The 3-chloro-1, 5-hexadiene content is 0.1 to 1.5%, and may be, for example, 0.1%, 0.2%, 0.5%, 0.8%, 1.0%, 1.2%, or 1.5%.
The cis-1, 3-dichloropropene may be 40 to 60%, for example, 40%, 42%, 45%, 48%, 50%, 50.5%, 52%, 58%, or 60%.
Trans-1, 3-dichloropropene may be 35 to 55%, for example, 35%, 38%, 40%, 41%, 42%, 45%, 46.5%, 48%, 50%, 52%, or 55%.
The content of 6-chloro-1-hexene is 0.5 to 2.5%, and may be, for example, 0.5%, 0.8%, 1.0%, 1.2%, 1.3%, 1.5%, 2.0%, 2.2%, or 2.5%.
Preferably, the first chlorination reaction unit comprises a chlorination reactor.
And a raw material inlet is arranged at the bottom of the chlorination reactor.
The chlorination reactor of the present invention is not particularly limited, and any reaction apparatus that can be used for chlorination reaction, which is well known to those skilled in the art, may be used, for example, a tank reactor or a tubular reactor.
Preferably, a condenser is arranged inside or outside the chlorination reactor.
Preferably, a first material storage device is arranged between the first chlorination reaction unit and the first rectification unit.
Preferably, a first material conveying device is arranged between the chlorination reactor and the first material storage device.
Preferably, a second material conveying device is arranged between the first material storage device and the first rectification unit.
Preferably, the first rectification unit comprises at least three rectification columns connected in series, preferably three rectification columns.
The utility model discloses preferably adopt the rectifying column of at least three grades series connection, wherein first order rectifying column is used for separating the heavy ends in the material, the heavy ends includes the organic matter that the number of carbon atoms is > 3, can be 3-chlorine-1, 5-hexadiene etc. for example. The second-stage rectifying tower and the third-stage rectifying tower are used for further separating cis-1, 3-dichloropropene and trans-1, 3-dichloropropene, so that the cis-1, 3-dichloropropene can further enter the second reaction unit for reaction.
Preferably, a material buffer device is arranged between each stage of rectifying tower.
Preferably, the material buffer device comprises a material buffer tank.
Preferably, the top of each stage of the rectifying tower is provided with an overhead condenser.
Preferably, the bottom of each stage of rectifying tower is provided with a tower kettle reboiler.
Preferably, the top discharge port of the previous stage rectifying tower is connected with the feed port of the next stage rectifying tower.
Preferably, the top of the first-stage rectifying tower is provided with a supplementary extraction outlet.
The supplementary extraction outlet is connected with a tower top reflux opening of the first-stage rectifying tower through a reflux conveying device;
the supplementary extraction outlet is also connected with a dichloropropane material extraction pipeline.
The utility model discloses the preferred dichloropropane material that sets up is adopted the pipeline and is in time adopted impurity dichloropropane material to finally improve the purity of trans-1, 3-dichloropropene.
Preferably, the system further comprises a component collecting device connected with the bottom of the first stage rectification column.
Preferably, the component collection means comprises a heavy component collection tank.
Preferably, the system device also comprises a trans-1, 3-chloropropene product storage device connected with the bottoms of the second-stage rectifying tower and the third-stage rectifying tower.
Preferably, the top discharge port of the third-stage rectifying tower is connected with the second reaction unit.
Preferably, a cis-1, 3-chloropropene storage device and a third material conveying device are further arranged between the first rectification unit and the second reaction unit.
Preferably, a discharge port at the top of the third-stage rectifying tower is connected with the cis-1, 3-chloropropene storage device firstly, and then is connected with the second reaction unit through the third material conveying device.
Preferably, the top of the separation and purification tower in the second rectification unit is connected with the cis-1, 3-chloropropene storage device, and then connected with the second reaction unit through the third material conveying device.
Preferably, a circulating material caching device and a circulating material conveying device are sequentially arranged outside the tower top of the separation and purification tower in the second rectifying unit.
The circulating material conveying device is connected with the cis-1, 3-chloropropene storage device.
Preferably, the second reaction unit comprises at least three stages of catalytic reaction devices connected in series.
And a material outlet of the last stage of catalytic reaction device is connected with the extraction reaction device.
Preferably, the catalytic reaction device comprises a photocatalytic reaction device and/or a thermocatalytic reaction device.
Preferably, the extraction reaction device is also separately connected with an extractant storage device.
Preferably, the upper part of the extraction reaction device is provided with a water phase outlet.
Preferably, the water phase outlet is connected with the water phase storage device through a fourth material conveying device.
Preferably, the second reaction unit further comprises a drying device connected to the bottom of the extraction reaction device.
The drying device is connected with the second rectifying unit.
The utility model discloses extraction reaction unit's bottom sets up drying device to get rid of the moisture in the chloropropene mixture after the extraction reaction, avoid the influence of follow-up rectification separation heavy moisture to the rectification.
Preferably, the drying device is a molecular sieve drying device.
The utility model discloses further preferred adoption molecular sieve drying device carries out the drying, can also further adsorb the inorganic impurity who remains in the chloropropene mixture, avoids the harmful effects to follow-up rectification.
Preferably, the drying device is connected with the second rectification unit through a fifth material conveying device.
Preferably, the bottom of the separation and purification tower in the second rectification unit is connected with a trans-1, 3-chloropropene product storage device.
The utility model discloses there is not special restriction to above-mentioned material storage device's form, structure and material, can adopt the nature, structure and the material to specific material that skilled person in the art is familiar, for example can be storage tank of 304 steel material etc..
The utility model discloses still do not have special restriction to above-mentioned material conveyor, can adopt any device that can be used to the material and carry that technical staff in the field are familiar, for example can be the pump etc. to the lectotype of pump also do not have special restriction, according to technological parameters such as the viscosity of material, flow demand carry on conventionally the lectotype can, also can adjust according to factory building and the specific condition of technology.
The operation method of the system device for continuously preparing trans-1, 3-dichloropropene comprises the following steps:
(1) conveying the reaction raw materials to a first chlorination reaction unit, carrying out chlorination reaction until the amount of 3-chloro-1, 5-hexadiene is reduced to be below 0.5%, and conveying the reaction raw materials to a first material storage device through a first material conveying device;
(2) the reacted materials are conveyed into a first-stage rectifying tower from a first material storage device through a second material conveying device, and are subjected to multistage rectification separation through the first-stage rectifying tower, a second-stage rectifying tower and a third-stage rectifying tower in sequence, and normal pressure rectification is adopted, wherein the tower bottom temperature is 100-120 ℃, and the tower top temperature is 100-120 ℃; or adopting negative pressure rectification, wherein the temperature at the bottom of the tower is less than 80 ℃, the temperature at the top of the tower is 54-60 ℃, and the pressure is-0.05 MPa to-0.08 MPa;
dichloropropane materials are extracted from the top of the first-stage rectifying tower, and heavy components at the bottom of the first-stage rectifying tower are conveyed to a component collecting device; trans-1, 3-dichloropropene with the mass fraction of more than or equal to 99 percent, which is obtained at the bottoms of the second-stage rectifying tower and the third-stage rectifying tower, is conveyed to a trans-1, 3-chloropropene product storage device;
(3) the cis-1, 3-dichloropropene with the mass fraction of more than 95 percent obtained at the top of the third-stage rectifying tower passes through a cis-1, 3-chloropropene storage device and then is conveyed to a catalytic reactor connected in series through a third material conveying device to carry out photocatalytic reaction or thermocatalytic reaction, so that the cis-1, 3-dichloropropene is converted into the trans-1, 3-dichloropropene, the reaction temperature is 30-100 ℃, the conversion rate is 30-50 percent, and a material after transposition reaction is obtained;
(4) mixing the transposition reaction material with a sodium sulfite solution in an extraction reaction device, stirring to remove redundant catalyst, extracting and layering, wherein the upper layer is a water phase, and the upper water phase enters a water phase storage device for recycling through a fourth material conveying device;
the lower-layer mixed chloropropene phase is conveyed into a drying device from the bottom to remove excessive water and inorganic impurities, then conveyed into a separation and purification tower of a second rectification unit for rectification and separation, and a trans-1, 3-chloropropene product with the mass fraction of more than 99 percent obtained at the bottom of the tower is conveyed into a trans-1, 3-chloropropene product storage device; and circularly conveying the cis-1, 3-chloropropene with the mass fraction of more than 95 percent obtained at the tower top into a cis-1, 3-chloropropene storage device to continue to enter a second reaction unit for reaction.
Compared with the prior art, the utility model discloses following beneficial effect has at least:
(1) the system device for continuously preparing trans-1, 3-dichloropropene provided by the utility model can chlorinate DD mixed agent, and can effectively separate high-purity cis-1, 3-dichloropropene and trans-1, 3-dichloropropene;
(2) the system device for continuously preparing trans-1, 3-dichloropropene provided by the utility model can realize the continuous conversion of DD mixed agent, and has high economic value; and the cis-1, 3-dichloropropene obtained by the catalytic reaction device through bromine free radical initiation separation is converted into trans-1, 3-dichloropropene with high added value and purity of more than 99 percent in situ, so that the operation is simple, the separation is easy, and the transposition efficiency is high.
Drawings
FIG. 1 is a diagram of a system for continuously preparing trans-1, 3-dichloropropene, which is provided by an embodiment of the invention.
In the figure: 1-a chlorination reactor; 21-a first stage rectification column; 22-a second stage rectification column; 23-a third stage rectification column; 31 to 33-catalytic reaction apparatus; 34-an extraction reaction device; 35-a drying device; 4-separation and purification tower; 51-54-tower bottom reboiler; 60-a circulating material buffer device; 61-a first material storage device; 62-a component collection device; a 63-dichloropropane material storage device; 64-65-a material buffer device between each level of rectifying tower; a 66-cis-1, 3-chloropropene storage device; a storage device for 67-trans-1, 3-chloropropene products; 68-aqueous phase storage; 69-extractant storage means; 71-74-a tower top condenser; 81-a first material conveying device; 82-second material conveying device; 83-third material conveying device; 84-a fourth material conveying device; 85-a fifth material conveying device; 86-87-material conveying devices between each stage of rectifying tower; 88-an extractant delivery device; 89-circulating material conveying device.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments with reference to the accompanying drawings.
The present invention will be described in further detail below. However, the following examples are only simple examples of the present invention, and do not represent or limit the scope of the present invention, which is defined by the appended claims.
It is to be understood that in the description of the present invention, the terms "central," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientation or positional relationship indicated in the drawings for the purpose of convenience and simplicity of description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
It should be noted that, unless explicitly stated or limited otherwise, the terms "disposed," "connected" and "connected" in the description of the present invention are to be construed broadly, and may for example be fixedly connected, detachably connected or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
It should be understood that the technical personnel in the field should understand that the utility model discloses in must include the necessary pipeline, conventional valve and the general pump equipment that are used for realizing the complete of technology, nevertheless do not belong to above the utility model discloses a main utility model point, technical personnel in the field can advance to add the overall arrangement by oneself based on process flow and equipment structure lectotype, the utility model discloses do not have special requirement and specific limit to this.
As a specific embodiment of the present invention, there is provided a system apparatus for continuously preparing trans-1, 3-dichloropropene, as shown in fig. 1, the system apparatus comprises a first chlorination reaction unit, a first rectification unit, a second reaction unit and a second rectification unit, which are connected in sequence.
The first chlorination reaction unit includes a chlorination reactor 1. A raw material inlet is arranged at the bottom of the chlorination reactor 1. The chlorination reactor 1 is internally or externally provided with a condenser. A first material storage device 61 is arranged between the first chlorination reaction unit and the first rectification unit. A first material conveying device 81 is arranged between the chlorination reactor 1 and the first material storage device 61. A second material conveying device 82 is arranged between the first material storage device 61 and the first rectification unit.
The first rectifying unit comprises three rectifying towers connected in series. And a material caching device is arranged between each stage of rectifying tower. The material caching device comprises a material caching tank. And a tower top condenser is arranged at the top of each stage of rectifying tower. The bottom of each stage of rectifying tower is provided with a tower kettle reboiler. The discharge hole at the top of the front stage of rectifying tower is connected with the feed inlet of the rear stage of rectifying tower. The top of the first-stage rectifying tower 21 is provided with a supplementary extraction outlet. The supplementary extraction outlet is connected with the tower top reflux port of the first-stage rectifying tower 21 through a reflux conveying device; the supplementary extraction outlet is also connected with a dichloropropane material extraction pipeline, and the dichloropropane material extraction pipeline is connected with a dichloropropane material storage device 63. And a discharge port at the top of the third-stage rectifying tower 23 is connected with the second reaction unit.
The system apparatus further includes a component collecting apparatus 62 connected to the bottom of the first-stage rectifying tower 21. The component collecting means 62 comprises a heavy component collecting tank. The system device also comprises a trans-1, 3-chloropropene product storage device 65 connected with the bottoms of the second-stage rectifying tower 22 and the third-stage rectifying tower 23.
A cis-1, 3-chloropropene storage device 64 and a third material conveying device 83 are also arranged between the first rectification unit and the second reaction unit. And a discharge port at the top of the third-stage rectifying tower 23 is connected with the cis-1, 3-chloropropene storage device 64 and then connected with the second reaction unit through the third material conveying device 83.
The second reaction unit comprises a catalytic reaction device and an extraction reaction device 34 which are connected in sequence; the second reaction unit comprises at least three stages of catalytic reaction devices connected in series. The material outlet of the last stage catalytic reaction device is connected with the extraction reaction device 34. The catalytic reaction device comprises a photocatalytic reaction device and/or a thermal catalytic reaction device. The extraction reaction device 34 is also separately connected with an extractant storage device 69; an extractant conveying device 88 is arranged between the extractant storage device 69 and the extraction reaction device 34. The upper part of the extraction reaction device 34 is provided with a water phase outlet. The aqueous phase outlet is connected to the aqueous phase storage means 68 via a fourth material transfer means 84.
The second reaction unit further includes a drying device 35 connected to the bottom of the extraction reaction device 34. The drying device 35 is connected to the second rectification unit. The drying device 35 is a molecular sieve drying device 35. The drying device 35 is connected to the second rectification unit via a fifth material conveying device 85.
The bottom of the separation and purification tower 4 in the second rectification unit is connected with a trans-1, 3-chloropropene product storage device 65. And the top of the separation and purification tower 4 in the second rectifying unit is connected with the inlet of the second reaction unit. The top of the separation and purification tower 4 in the second rectification unit sequentially passes through a circulating material caching device 60, a circulating material conveying device 89 and the cis-1, 3-chloropropene storage device 64, and is connected with the second reaction unit through the third material conveying device 83.
Application example 1
The application example provides a method for continuously preparing trans-1, 3-dichloropropene, which is carried out by adopting the system device for continuously preparing trans-1, 3-dichloropropene, provided by the above specific embodiment, and specifically comprises the following steps:
(1) the DD mixing agent (the concrete components are, by mass, 5% of 1, 2-dichloropropane, 0.8% of 3, 3-dichloropropene, 0.7% of 3-chloro-1, 5-hexadiene, 48.5% of cis-1, 3-dichloropropene, 44.5% of trans-1, 3-dichloropropene and 1.3% of 6-chloro-1-hexene) is conveyed into a chlorination reactor 1, chlorine gas is introduced at the temperature of 0 ℃ controlled by a condenser, the flow of the chlorine gas is controlled at 60L/h, chlorination reaction is carried out, a central control sample is taken for gas chromatography detection in the reaction, and when the amount of the 3-chloro-1, 5-hexadiene is reduced to be below 0.5%, the mixed agent is conveyed into a first material storage device 61 by a first material conveying device 81;
(2) the reacted materials are conveyed from the first material storage device 61 to the first-stage rectifying tower 21 through the second material conveying device 82, and are sequentially subjected to multi-stage rectification separation through the first-stage rectifying tower 21, the second-stage rectifying tower 22 and the third-stage rectifying tower 23, wherein negative pressure rectification of-0.075 MPa is adopted, wherein the tower bottom temperature is 75 ℃, the tower top temperature is 54-60 ℃, the reflux ratio is 3-5: 1, and the transition fraction is conveyed to the rectifying tower again through a reflux pump for re-separation;
dichloropropane materials are extracted from the top of the first-stage rectifying tower 21, and heavy components at the bottom of the first-stage rectifying tower are conveyed to a component collecting device 62; trans-1, 3-dichloropropene with the mass fraction of more than or equal to 99 percent, which is obtained at the bottoms of the second-stage rectifying tower 22 and the third-stage rectifying tower 23, is conveyed to a trans-1, 3-chloropropene product storage device 65;
(3) the cis-1, 3-dichloropropene obtained at the top of the third-stage rectifying tower 23 with the mass fraction of more than 95 percent passes through a cis-1, 3-chloropropene storage device 64 and then is conveyed into a catalytic reactor connected in series through a third material conveying device 83 for photocatalytic reaction, a light source is a full-spectrum LED lamp, a catalyst is bromine, the total amount of the bromine is 0.5wt percent of 1, 3-dichloropropene, the reaction temperature is 50 ℃, the cis-1, 3-dichloropropene is converted into the trans-1, 3-dichloropropene, the conversion rate is 45 percent, the selectivity is more than 99 percent, and a material after transposition reaction is obtained;
(4) mixing the transposition reaction material with a saturated sodium sulfite solution in the extraction reaction device 34, stirring to remove redundant catalyst, extracting and layering, wherein the upper layer is a water phase, and the upper water phase enters a water phase storage device 68 for recycling through a fourth material conveying device 84;
the lower-layer mixed chloropropene phase is fed into a drying device 35 from the bottom to remove excessive water and inorganic impurities, then is fed into a separation and purification tower 4 of a second rectification unit for rectification and separation, and a trans-1, 3-chloropropene product with the mass fraction of more than 99 percent obtained at the bottom of the tower is fed into a trans-1, 3-chloropropene product storage device 65; the cis-1, 3-chloropropene with the mass fraction of more than 95 percent obtained at the tower top is circularly sent into a cis-1, 3-chloropropene storage device 64 to continue to enter the second reaction unit for reaction.
Application example 2
The application example provides a method for continuously preparing trans-1, 3-dichloropropene, which is carried out by adopting the system device for continuously preparing trans-1, 3-dichloropropene, provided by the above specific embodiment, and specifically comprises the following steps:
(1) the DD mixing agent (the concrete components are, by mass, 20% of 1, 2-dichloropropane, 1% of 3, 3-dichloropropene, 0.8% of 3-chloro-1, 5-hexadiene, 40.5% of cis-1, 3-dichloropropene, 36.5% of trans-1, 3-dichloropropene and 1.3% of 6-chloro-1-hexene) is conveyed into a chlorination reactor 1, chlorine gas is introduced while the reaction is carried out at the temperature of 5 ℃ by using a condenser, the flow rate of the chlorine gas is controlled at 30L/h, the reaction is carried out at the stirring speed of 300r/min, a central control sample is taken for gas chromatography detection, and when the amount of the 3-chloro-1, 5-hexadiene is reduced to be below 0.5%, the mixed agent is conveyed into a first material storage device 61 by a first material conveying device 81;
(2) the reacted materials are conveyed from the first material storage device 61 to the first-stage rectifying tower 21 through the second material conveying device 82, and are sequentially subjected to multi-stage rectification separation through the first-stage rectifying tower 21, the second-stage rectifying tower 22 and the third-stage rectifying tower 23, wherein negative pressure rectification of-0.008 MPa is adopted, wherein the tower bottom temperature is 78 ℃, the tower top temperature is 54-60 ℃, the reflux ratio is 3.5-5: 1, and the transition fraction is conveyed to the rectifying tower again through a reflux pump for re-separation;
dichloropropane materials are extracted from the top of the first-stage rectifying tower 21, and heavy components at the bottom of the first-stage rectifying tower are conveyed to a component collecting device 62; trans-1, 3-dichloropropene with the mass fraction of more than or equal to 99 percent, which is obtained at the bottoms of the second-stage rectifying tower 22 and the third-stage rectifying tower 23, is conveyed to a trans-1, 3-chloropropene product storage device 65;
(3) the cis-1, 3-dichloropropene obtained at the top of the third-stage rectifying tower 23 with the mass fraction of more than 95 percent passes through a cis-1, 3-chloropropene storage device 64 and then is conveyed to a catalytic reactor connected in series through a third material conveying device 83 for carrying out thermocatalytic reaction, the catalyst is bromine, the total amount of the bromine is 0.5wt percent of 1, 3-dichloropropene, the reaction temperature is 50 ℃, the cis-1, 3-dichloropropene is converted into the trans-1, 3-dichloropropene, the conversion rate is 30 percent, the selectivity is more than 99 percent, and a material after transposition reaction is obtained;
(4) mixing the transposition reaction material with 0.25 wt% of sodium sulfite solution in the extraction reaction device 34, stirring to remove redundant catalyst, extracting and layering, wherein the upper layer is a water phase, and the upper water phase enters a water phase storage device 68 for recycling through a fourth material conveying device 84;
the lower-layer mixed chloropropene phase is fed into a drying device 35 from the bottom to remove excessive water and inorganic impurities, then is fed into a separation and purification tower 4 of a second rectification unit for rectification and separation, and a trans-1, 3-chloropropene product with the mass fraction of more than 99 percent obtained at the bottom of the tower is fed into a trans-1, 3-chloropropene product storage device 65; the cis-1, 3-chloropropene with the mass fraction of more than 95 percent obtained at the tower top is circularly sent into a cis-1, 3-chloropropene storage device 64 to continue to enter the second reaction unit for reaction.
Application example 3
The application example provides a method for continuously preparing trans-1, 3-dichloropropene, which is carried out by adopting the system device for continuously preparing trans-1, 3-dichloropropene, provided by the above specific embodiment, and specifically comprises the following steps:
(1) the DD mixing agent (the concrete components are, by mass, 0.2% of 1, 2-dichloropropane, 1% of 3, 3-dichloropropene, 0.8% of 3-chloro-1, 5-hexadiene, 50.5% of cis-1, 3-dichloropropene, 46.5% of trans-1, 3-dichloropropene and 1.3% of 6-chloro-1-hexene) is conveyed into a chlorination reactor 1, chlorine gas is started to be introduced by using a condenser to control the temperature to be 3 ℃, the flow rate of the chlorine gas is controlled to be 40L/h, stirring is carried out while reacting at the stirring speed of 300rpm/min, chlorination reaction is carried out, a central sample control gas chromatography is taken out for detection, and when the amount of the 3-chloro-1, 5-hexadiene is reduced to be below 0.05%, the mixed agent is conveyed into a first material storage device 61 through a first material conveying device 81;
(2) the reacted materials are conveyed from the first material storage device 61 to the first-stage rectifying tower 21 through the second material conveying device 82, and are sequentially subjected to multi-stage rectification separation through the first-stage rectifying tower 21, the second-stage rectifying tower 22 and the third-stage rectifying tower 23, wherein normal pressure rectification is adopted, the tower bottom temperature is 110-115 ℃, the tower top temperature is 105-120 ℃, the reflux ratio is 3-5: 1, and the transition fraction is conveyed to the rectifying tower again through a reflux pump for re-separation;
dichloropropane materials are extracted from the top of the first-stage rectifying tower 21, and heavy components at the bottom of the first-stage rectifying tower are conveyed to a component collecting device 62; trans-1, 3-dichloropropene with the mass fraction of more than or equal to 99 percent, which is obtained at the bottoms of the second-stage rectifying tower 22 and the third-stage rectifying tower 23, is conveyed to a trans-1, 3-chloropropene product storage device 65;
(3) the cis-1, 3-dichloropropene obtained at the top of the third-stage rectifying tower 23 with the mass fraction of more than 95 percent passes through a cis-1, 3-chloropropene storage device 64 and then is conveyed to a catalytic reactor connected in series through a third material conveying device 83 for a thermal catalytic reaction, the catalyst is iodine, the total amount of iodine is 1wt percent of 1, 3-dichloropropene, the reaction temperature is 50 ℃, the cis-1, 3-dichloropropene is converted into the trans-1, 3-dichloropropene, the conversion rate is 40 percent, and the selectivity is more than 99 percent, so that a material after the transposition reaction is obtained;
(4) mixing the transposition reaction material with a saturated sodium sulfite solution in the extraction reaction device 34, stirring to remove redundant catalyst, extracting and layering, wherein the upper layer is a water phase, and the upper water phase enters a water phase storage device 68 for recycling through a fourth material conveying device 84;
the lower-layer mixed chloropropene phase is fed into a drying device 35 from the bottom to remove excessive water and inorganic impurities, then is fed into a separation and purification tower 4 of a second rectification unit for rectification and separation, and a trans-1, 3-chloropropene product with the mass fraction of more than 99 percent obtained at the bottom of the tower is fed into a trans-1, 3-chloropropene product storage device 65; the cis-1, 3-chloropropene with the mass fraction of more than 95 percent obtained at the tower top is circularly sent into a cis-1, 3-chloropropene storage device 64 to continue to enter the second reaction unit for reaction.
Application example 4
The application example provides a method for continuously preparing trans-1, 3-dichloropropene, which is carried out by adopting the system device for continuously preparing trans-1, 3-dichloropropene, provided by the above specific embodiment, and specifically comprises the following steps:
(1) the DD mixing agent (the concrete components are, by mass, 5% of 1, 2-dichloropropane, 1% of 3, 3-dichloropropene, 0.8% of 3-chloro-1, 5-hexadiene, 48.5% of cis-1, 3-dichloropropene, 44.5% of trans-1, 3-dichloropropene and 1.2% of 6-chloro-1-hexene) is conveyed into a chlorination reactor 1, the temperature is controlled at 8 ℃ by using a condenser, chlorine gas is introduced, the flow rate of the chlorine gas is controlled at 100L/h, chlorination reaction is carried out, a central sample control gas chromatography is taken in the reaction for detection, and when the amount of the 3-chloro-1, 5-hexadiene is reduced to be below 0.05%, the mixed agent is conveyed into a first material storage device 61 by a first material conveying device 81;
(2) the reacted materials are conveyed from the first material storage device 61 to the first-stage rectifying tower 21 through the second material conveying device 82, and are sequentially subjected to multi-stage rectification separation through the first-stage rectifying tower 21, the second-stage rectifying tower 22 and the third-stage rectifying tower 23, wherein negative pressure rectification of-0.075 MPa is adopted, wherein the tower bottom temperature is 70 ℃, the tower top temperature is 55-60 ℃, the reflux ratio is 3-4: 1, and the transition fraction is conveyed to the rectifying tower again through a reflux pump for re-separation;
dichloropropane materials are extracted from the top of the first-stage rectifying tower 21, and heavy components at the bottom of the first-stage rectifying tower are conveyed to a component collecting device 62; trans-1, 3-dichloropropene with the mass fraction of more than or equal to 99 percent, which is obtained at the bottoms of the second-stage rectifying tower 22 and the third-stage rectifying tower 23, is conveyed to a trans-1, 3-chloropropene product storage device 65;
(3) the cis-1, 3-dichloropropene obtained at the top of the third-stage rectifying tower 23 with the mass fraction of more than 95 percent passes through a cis-1, 3-chloropropene storage device 64 and then is conveyed into a catalytic reactor connected in series through a third material conveying device 83 for photocatalytic reaction, the light source is a high-pressure mercury lamp, the catalyst is bromine, the total amount of the bromine is 1wt percent of the 1, 3-dichloropropene, the reaction temperature is 70 ℃, the cis-1, 3-dichloropropene is converted into the trans-1, 3-dichloropropene, the conversion rate is 50 percent, the selectivity is more than 99 percent, and a material after transposition reaction is obtained;
(4) mixing the transposition reaction material with a saturated sodium sulfite solution in the extraction reaction device 34, stirring to remove redundant catalyst, extracting and layering, wherein the upper layer is a water phase, and the upper water phase enters a water phase storage device 68 for recycling through a fourth material conveying device 84;
the lower-layer mixed chloropropene phase is fed into a drying device 35 from the bottom to remove excessive water and inorganic impurities, then is fed into a separation and purification tower 4 of a second rectification unit for rectification and separation, and a trans-1, 3-chloropropene product with the mass fraction of more than 99 percent obtained at the bottom of the tower is fed into a trans-1, 3-chloropropene product storage device 65; the cis-1, 3-chloropropene with the mass fraction of more than 95 percent obtained at the tower top is circularly sent into a cis-1, 3-chloropropene storage device 64 to continue to enter the second reaction unit for reaction.
In the above process, the system device is operated continuously for a long time, so that some parameters are controlled within a range.
To sum up, the utility model provides a system's device of serialization preparation trans-1, 3-dichloropropene can serialization turns into the mixed agent of DD trans-1, 3-chloropropene that the purity is greater than 99%, is showing and is improving chloropropene low reaches product added value.
The applicant states that the present invention is described by the above embodiments, but the present invention is not limited to the above detailed structural features, i.e. the present invention can be implemented only by relying on the above detailed structural features. It should be clear to those skilled in the art that any modifications to the present invention, to the equivalent replacement of selected parts and the addition of auxiliary parts, the selection of specific modes, etc., all fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. A system device for continuously preparing trans-1, 3-dichloropropene is characterized by comprising a first chlorination reaction unit, a first rectification unit, a second reaction unit and a second rectification unit which are sequentially connected;
the second reaction unit comprises a catalytic reaction device and an extraction reaction device which are connected in sequence;
and the top of the separation and purification tower in the second rectifying unit is connected with the inlet of the second reaction unit.
2. The system for continuously preparing trans-1, 3-dichloropropene according to claim 1, wherein the first chlorination reaction unit comprises a chlorination reactor;
and a raw material inlet is arranged at the bottom of the chlorination reactor.
3. The system device for continuously preparing trans-1, 3-dichloropropene according to claim 1, wherein the first rectification unit comprises at least three rectification columns connected in series.
4. The system device for continuously preparing trans-1, 3-dichloropropene according to claim 3, wherein a material buffer device is arranged between each stage of rectifying tower.
5. The system device for continuously preparing trans-1, 3-dichloropropene according to claim 3 or 4, wherein the top of the first-stage rectifying tower is provided with a supplementary extraction outlet;
the supplementary extraction outlet is connected with a tower top reflux opening of the first-stage rectifying tower through a reflux conveying device;
the supplementary extraction outlet is also connected with a dichloropropane material extraction pipeline.
6. The system for continuously preparing trans-1, 3-dichloropropene according to claim 3 or 4, wherein the system further comprises a component collecting device connected with the bottom of the first-stage rectification tower.
7. The system for continuously preparing trans-1, 3-dichloropropene according to claim 3 or 4, wherein the system also comprises a trans-1, 3-chloropropene product storage device connected with the bottoms of the second-stage rectifying tower and the third-stage rectifying tower.
8. The system device for continuously preparing trans-1, 3-dichloropropene according to claim 1, wherein the second reaction unit comprises at least three catalytic reaction devices connected in series;
and a material outlet of the last stage of catalytic reaction device is connected with the extraction reaction device.
9. The system for continuously preparing trans-1, 3-dichloropropene according to claim 1 or 2, wherein the second reaction unit further comprises a drying device connected with the bottom of the extraction reaction device;
the drying device is connected with the second rectifying unit.
10. The system device for continuously preparing trans-1, 3-dichloropropene according to claim 7, wherein the bottom of the separation and purification tower in the second rectification unit is connected with a trans-1, 3-chloropropene product storage device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122451468.0U CN216005719U (en) | 2021-10-12 | 2021-10-12 | System device for continuously preparing trans-1, 3-dichloropropene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122451468.0U CN216005719U (en) | 2021-10-12 | 2021-10-12 | System device for continuously preparing trans-1, 3-dichloropropene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN216005719U true CN216005719U (en) | 2022-03-11 |
Family
ID=80521853
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202122451468.0U Active CN216005719U (en) | 2021-10-12 | 2021-10-12 | System device for continuously preparing trans-1, 3-dichloropropene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN216005719U (en) |
-
2021
- 2021-10-12 CN CN202122451468.0U patent/CN216005719U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0209768B1 (en) | Liquid phase chlorination of chlorinated methanes | |
| CN108840310B (en) | Device and process for producing hydrogen chloride by deep analysis from dilute hydrochloric acid | |
| CN101070140B (en) | Method for producing chlorine by coupling hydrogen chloride oxidation and dehydration | |
| KR102364284B1 (en) | Method for preparing high content 2-methylallyl chloride | |
| CN106892792B (en) | Continuous synthesis method and equipment of 3, 4-dichloro benzotrifluoride | |
| MXPA04011415A (en) | Method for producing isocyanates. | |
| CN216005719U (en) | System device for continuously preparing trans-1, 3-dichloropropene | |
| CN111574329A (en) | Reactive distillation device and method for producing 4-chloro-3, 5-dimethylphenol | |
| CN117105759A (en) | Method for continuously preparing 2-chloro-1- (1-chlorocyclopropyl) ethanone | |
| CN116063144A (en) | Method for producing 2, 4-dichlorotoluene | |
| CN113480461B (en) | Method for continuously synthesizing perchloromethyl mercaptan by utilizing reaction tower | |
| CN114315749B (en) | Method for synthesizing aliskiren intermediate by continuous flow microreactor | |
| CN111548248B (en) | Method for producing 1,3,3, 3-tetrachloropropene | |
| CN211284207U (en) | 2-chlorine-3-trifluoromethyl pyridine synthesizer | |
| CN112094171B (en) | Method for synthesizing m-chlorotoluene through isomerization reaction | |
| CN108409528B (en) | Novel process for preparing p-dichlorobenzene by adopting novel reaction equipment | |
| CN113549027A (en) | Continuous production process of 2-chloro-5-chloromethyl thiazole | |
| CN101367708B (en) | Preparation of chloro-cyclohexane under nitrogen protection | |
| CN116023257B (en) | Continuous production method of high-purity propionyl chloride | |
| CN116143582B (en) | Preparation method of p-chlorotoluene and o-chlorotoluene | |
| CN210974481U (en) | Device for improving concentration of phosgenation reaction phosgene | |
| CN216630761U (en) | Device for synthesizing methylbenzene through alkylation reaction | |
| CN116444341B (en) | Method for purifying p-chlorotoluene and o-chlorotoluene | |
| CN114436843B (en) | Method for continuously producing dimethyl adipate from cyclohexane | |
| CN112010736B (en) | Separation and recovery process of cyclohexanol process raw material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |