Ethephon continuous production method and production device

文档序号:548118 发布日期:2021-06-04 浏览:24次 中文

阅读说明:本技术 一种乙烯利连续生产方法及生产装置 (Ethephon continuous production method and production device ) 是由 黄金 李�杰 唐素荣 汪英瑞 姜育田 朱学军 陈建国 万金方 于同锋 于 2020-12-28 设计创作,主要内容包括:本发明公开了一种乙烯利连续生产方法及生产装置,启动所述转料泵和所述第二气泵,开启所述第三阀门和所述第一阀门,反应后的混合液通过所述内插管进入所述第一二级酸解釜,注入新鲜的氯化氢气体至所述第一二级酸解釜中,收集一公斤混合液后,开启所述第四阀门所述第三阀门,反应后的混合液通过所述内插管进入所述第二二级酸解釜,并注入新鲜的氯化氢气体至所述第二二级酸解釜中,在所述气液分离罐中分离从所述管式反应器产生的尾气和副产二氯乙烷及过量的氯化氢,通过所述排气管将所述气液分离罐中的气体排到所述尾气吸收釜进行收集,通过上述结构的设置实现便于技术人员处理乙烯利生产时所产生的尾气及副产二氯乙烷气体。(The invention discloses a continuous ethephon production method and a continuous ethephon production device, wherein a material transferring pump and a second air pump are started, a third valve and a first valve are opened, a mixed solution after reaction enters a first secondary acidolysis kettle through an inner insertion pipe, fresh hydrogen chloride gas is injected into the first secondary acidolysis kettle, a fourth valve and the third valve are opened after one kilogram of mixed solution is collected, the mixed solution after reaction enters a second secondary acidolysis kettle through the inner insertion pipe and is injected into the second secondary acidolysis kettle, tail gas, byproduct dichloroethane and excessive hydrogen chloride generated from a tubular reactor are separated in a gas-liquid separation tank, gas in the gas-liquid separation tank is discharged to a tail gas absorption kettle through an exhaust pipe for collection, and the tail gas and byproduct dichloroethane gas generated during ethephon production can be conveniently treated by technical personnel through the arrangement of the structure.)

1. A continuous production device for ethephon, which is characterized in that,

comprises a material storage tank, a gas storage tank, a transportation component, a tubular reactor, an outer cannula, a gas-liquid separation tank, a transportation component, a control component, a first secondary acidolysis tank, a second secondary acidolysis tank, an air inlet pipe, an absorption component, a gas circulation pipe, a first air pump, a first valve and a second valve, wherein one end of the transportation component is communicated with the material storage tank and the gas storage tank respectively, the other end of the transportation component is communicated with the bottom of the tubular reactor, one end of the outer cannula is communicated with the top of the tubular reactor, the other end of the outer cannula is communicated with the gas-liquid separation tank, one end of the transportation component penetrates through the bottom of the tubular reactor, the other end of the transportation component is communicated with the bottom of the first secondary acidolysis tank and the bottom of the second secondary acidolysis tank respectively, and the control component penetrates through the transportation component, the one end of intake pipe with the gas-liquid separation jar intercommunication, the other end of intake pipe respectively with first second grade acidolysis cauldron with second grade acidolysis cauldron intercommunication, the absorption subassembly with the gas-liquid separation jar intercommunication, the one end of gas flow tube with the jar intercommunication is deposited to the gas, the other end of gas flow tube respectively with first second grade acidolysis cauldron with second grade acidolysis cauldron intercommunication, first valve runs through the lateral wall of gas flow tube, and be close to first second grade acidolysis cauldron, the second valve runs through the lateral wall of gas flow tube, and be close to second grade acidolysis cauldron.

2. The apparatus for continuous production of ethephon according to claim 1,

the transportation assembly comprises a first transportation pipe and a material transferring pump, one end of the first transportation pipe is communicated with the material storage tank, the other end of the first transportation pipe is communicated with the bottom of the tubular reactor, and the material transferring pump penetrates through the outer side wall of the first transportation pipe.

3. The apparatus for continuous production of ethephon according to claim 2,

the transportation assembly further comprises a second transportation pipe and a second air pump, one end of the second transportation pipe is communicated with the gas storage tank, the other end of the second transportation pipe is communicated with the first transportation pipe, and the second air pump penetrates through the outer side wall of the second transportation pipe.

4. The apparatus for continuous production of ethephon according to claim 3,

the control assembly comprises a third valve and a fourth valve, and the third valve and the fourth valve respectively penetrate through the conveying assembly.

5. The apparatus for continuous production of ethephon according to claim 4,

the conveying assembly comprises an inner inserting pipe, a first branch pipe and a second branch pipe, one end of the inner inserting pipe penetrates through the bottom of the tubular reactor, the other end of the inner inserting pipe is communicated with the first branch pipe and the second branch pipe respectively, the first branch pipe is communicated with the bottom of the first secondary acidolysis kettle, the second branch pipe is communicated with the bottom of the second secondary acidolysis kettle, the third valve penetrates through the outer side wall of the first branch pipe, and the fourth valve penetrates through the outer side wall of the second branch pipe.

6. The apparatus for continuous production of ethephon according to claim 5,

the absorption assembly comprises an exhaust pipe and a tail gas absorption kettle, one end of the exhaust pipe is communicated with the gas-liquid separation tank, and the other end of the exhaust pipe is communicated with the tail gas absorption kettle.

7. A process for the continuous production of ethephon using the continuous production apparatus for ethephon according to claim 6, comprising the steps of:

starting the material transfer pump to transport 2-chloroethylphosphonic acid bis- (2-chloroethyl) ester from the material storage tank through the first transport pipe into the tubular reactor;

starting the second air pump, conveying fresh hydrogen chloride gas from the gas storage tank into the tubular reactor through the second conveying pipe, and continuously reacting with 2-chloroethyl phosphonic acid bis- (2-chloroethyl) ester;

opening the third valve and the first valve, closing the fourth valve and the third valve, allowing the reacted mixed solution to enter the first secondary acidolysis kettle through the inner insertion tube, starting the first air pump, and injecting fresh hydrogen chloride gas into the first secondary acidolysis kettle;

after one kilogram of mixed liquid is collected, the third valve and the first valve are closed, the fourth valve and the third valve are opened, the mixed liquid after reaction enters the second-stage acidolysis kettle through the inner insertion pipe, the first air pump is started, and fresh hydrogen chloride gas is injected into the second-stage acidolysis kettle;

separating the tail gas and byproduct dichloroethane generated from the tubular reactor and the excessive hydrogen chloride in the first secondary acidolysis kettle and the second secondary acidolysis kettle in the gas-liquid separation tank;

and discharging the gas in the gas-liquid separation tank to the tail gas absorption kettle through the exhaust pipe for collection.

Technical Field

The invention relates to the technical field of ethephon production, in particular to a method and a device for continuously producing ethephon.

Background

Ethephon, molecular weight 144.50, is an organic compound, pure white needle crystal, light brown liquid, soluble in water, methanol, acetone, ethylene glycol, and propylene glycol, slightly soluble in toluene, insoluble in petroleum ether, and used as growth stimulator for agricultural plants. Ethephon is a high-quality and high-efficiency plant growth regulator, and has the effects of promoting fruit ripening, stimulating wound flow, regulating the sex transformation of partial plants and the like.

At present, a large amount of tail gas and byproducts are generated in the process of producing ethephon, and technicians are inconvenient to treat the tail gas and the byproduct dichloroethane gas which are generated subsequently.

Disclosure of Invention

The invention aims to provide a method and a device for continuously producing ethephon, and aims to solve the technical problem that technicians in the prior art are inconvenient to treat tail gas and byproduct dichloroethane gas generated in ethephon production.

In order to achieve the purpose, the invention adopts a continuous ethephon production device, which comprises a material storage tank, a gas storage tank, a transportation component, a tubular reactor, an outer insertion pipe, a gas-liquid separation tank, a transportation component, a control component, a first secondary acidolysis kettle, a second secondary acidolysis kettle, a gas inlet pipe, an absorption component, a gas circulation pipe, a first gas pump, a first valve and a second valve, wherein one end of the transportation component is respectively communicated with the material storage tank and the gas storage tank, the other end of the transportation component is communicated with the bottom of the tubular reactor, one end of the outer insertion pipe is communicated with the top of the tubular reactor, the other end of the outer insertion pipe is communicated with the gas-liquid separation tank, one end of the transportation component penetrates through the bottom of the tubular reactor, the other end of the transportation component is respectively communicated with the bottom of the first secondary acidolysis kettle and the bottom of the second secondary acidolysis kettle, the control assembly runs through conveying assembly, the one end of intake pipe with gas-liquid separation jar intercommunication, the other end of intake pipe respectively with first second grade acidolysis cauldron with second grade acidolysis cauldron intercommunication, absorption assembly with gas-liquid separation jar intercommunication, the one end of gas runner pipe with jar intercommunication is deposited to the gas, the other end of gas runner pipe respectively with first second grade acidolysis cauldron with second grade acidolysis cauldron intercommunication, first valve runs through the lateral wall of gas runner pipe, and is close to first second grade acidolysis cauldron, the second valve runs through the lateral wall of gas runner pipe, and is close to second grade acidolysis cauldron.

The conveying assembly comprises a first conveying pipe and a material transferring pump, one end of the first conveying pipe is communicated with the material storage tank, the other end of the first conveying pipe is communicated with the bottom of the tubular reactor, and the material transferring pump penetrates through the outer side wall of the first conveying pipe.

The transportation assembly further comprises a second transportation pipe and a second air pump, one end of the second transportation pipe is communicated with the gas storage tank, the other end of the second transportation pipe is communicated with the first transportation pipe, and the second air pump penetrates through the outer side wall of the second transportation pipe.

Wherein, the control assembly comprises a third valve and a fourth valve, and the third valve and the fourth valve respectively penetrate through the conveying assembly.

The conveying assembly comprises an inner inserting pipe, a first branch pipe and a second branch pipe, one end of the inner inserting pipe penetrates through the bottom of the tubular reactor, the other end of the inner inserting pipe is communicated with the first branch pipe and the second branch pipe respectively, the first branch pipe is communicated with the bottom of the first secondary acidolysis kettle, the second branch pipe is communicated with the bottom of the second secondary acidolysis kettle, the third valve penetrates through the outer side wall of the first branch pipe, and the fourth valve penetrates through the outer side wall of the second branch pipe.

The absorption assembly comprises an exhaust pipe and a tail gas absorption kettle, one end of the exhaust pipe is communicated with the gas-liquid separation tank, and the other end of the exhaust pipe is communicated with the tail gas absorption kettle.

The invention also provides a continuous ethephon production method adopting the continuous ethephon production device, which comprises the following steps:

starting the material transfer pump to transport 2-chloroethylphosphonic acid bis- (2-chloroethyl) ester from the material storage tank through the first transport pipe into the tubular reactor;

starting the second air pump, conveying fresh hydrogen chloride gas from the gas storage tank into the tubular reactor through the second conveying pipe, and continuously reacting with 2-chloroethyl phosphonic acid bis- (2-chloroethyl) ester;

opening the third valve and the first valve, closing the fourth valve and the third valve, allowing the reacted mixed solution to enter the first secondary acidolysis kettle through the inner insertion tube, starting the first air pump, and injecting fresh hydrogen chloride gas into the first secondary acidolysis kettle;

after one kilogram of mixed liquid is collected, the third valve and the first valve are closed, the fourth valve and the third valve are opened, the mixed liquid after reaction enters the second-stage acidolysis kettle through the inner insertion pipe, the first air pump is started, and fresh hydrogen chloride gas is injected into the second-stage acidolysis kettle;

separating the tail gas and byproduct dichloroethane generated from the tubular reactor and the excessive hydrogen chloride in the first secondary acidolysis kettle and the second secondary acidolysis kettle in the gas-liquid separation tank;

and discharging the gas in the gas-liquid separation tank to the tail gas absorption kettle through the exhaust pipe for collection.

The invention has the beneficial effects that: when a technician uses the 2-chloroethyl bis- (2-chloroethyl) phosphonate to prepare ethephon, the 2-chloroethyl bis- (2-chloroethyl) phosphonate is placed in the material storage tank, hydrogen chloride gas is placed in the gas storage tank, and the 2-chloroethyl bis- (2-chloroethyl) phosphonate and the hydrogen chloride gas are respectively fed forward from the bottom of the tubular reactor to the tubular reactor for reaction through the transportation component, wherein the molar ratio of the hydrogen chloride to the 2-chloroethyl bis- (2-chloroethyl) phosphonate is 2-2.5: 1, reducing the consumption of raw materials and reducing the amount of tail gas and byproducts, controlling the pressure in the tubular reactor to be 0.1-0.5MPa and the temperature to be 120-200 ℃, and extracting excessive tail gas and byproduct dichloroethane from the top of the tubular reactor to the gas-liquid separation tank; meanwhile, the reaction mixed liquid of the 2-chloroethyl phosphonic acid di- (2-chloroethyl) ester and the hydrogen chloride gas in the tubular reactor respectively enters the first secondary acidolysis kettle and the second secondary acidolysis kettle through a conveying component, the first air pump is controlled, the third valve and the fourth valve are adjusted according to the working states of the first secondary acidolysis kettle and the second secondary acidolysis kettle, fresh hydrogen chloride gas is injected into the first secondary acidolysis kettle and the second secondary acidolysis kettle, the pressure in the first secondary acidolysis kettle and the pressure in the second secondary acidolysis kettle are both controlled to be 0.1-0.5MPa, the temperature is both controlled to be 120-degree centigrade, the excessive hydrogen chloride gas and byproduct dichloroethane in the first secondary acidolysis kettle and the second secondary acidolysis kettle, and the tail gas and byproduct dichloroethane generated in the tubular reactor enter the gas-liquid separation tank together for separation, the gas absorption assembly is used for absorption treatment, the consumption of hydrogen chloride is reduced, the quality of ethephon products is improved, and the tail gas and the byproduct dichloroethane gas generated by the technicians during ethephon production are conveniently treated.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a flow chart of the steps of the process for the continuous production of ethephon according to the present invention.

FIG. 2 is a schematic view of the structure of a continuous production apparatus for ethephon of the present invention.

FIG. 3 is a schematic view showing a part of the apparatus for continuous production of ethephon according to the present invention.

FIG. 4 is a schematic view showing the structure of another part of the apparatus for continuous production of ethephon according to the present invention.

Fig. 5 is an enlarged view of a portion of the structure of fig. 3 according to the present invention.

FIG. 6 is a schematic view of the structure of the tubular reactor of the present invention.

FIG. 7 is a side view of a tubular reactor of the present invention.

Fig. 8 is a schematic structural view of the junction of the column of the present invention and the packing placement frame.

1-material storage tank, 2-gas storage tank, 3-transportation component, 4-tubular reactor, 5-external insertion tube, 6-gas-liquid separation tank, 7-transportation component, 8-control component, 9-first second-stage acidolysis kettle, 10-second-stage acidolysis kettle, 11-gas inlet tube, 12-absorption component, 13-gas circulation tube, 14-first gas pump, 15-first valve, 16-second valve, 17-installation groove, 18-holding groove, 19-exhaust tube, 20-tail gas absorption kettle, 31-first transportation tube, 32-material transfer pump, 33-second transportation tube, 34-second gas pump, 41-column body, 42-connection cover, 43-glass filler, 44-filler placing rack, 45-abutting assembly, 46-sealing strip, 47-extension spring, 48-abutting block, 49-pulling strip, 71-inner insertion tube, 72-first branch tube, 73-second branch tube, 81-third valve and 82-fourth valve.

Detailed Description

Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.

In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.

Referring to fig. 2 to 8, the present invention provides a continuous ethephon production apparatus, which comprises a material storage tank 1, a gas storage tank 2, a transportation component 3, a tubular reactor 4, an outer cannula 5, a gas-liquid separation tank 6, a transportation component 7, a control component 8, a first secondary acidolysis tank 9, a second secondary acidolysis tank 10, a gas inlet pipe 11, an absorption component 12, a gas circulation pipe 13, a first gas pump 14, a first valve 15 and a second valve 16, wherein one end of the transportation component 3 is respectively communicated with the material storage tank 1 and the gas storage tank 2, the other end of the transportation component 3 is communicated with the bottom of the tubular reactor 4, one end of the outer cannula 5 is communicated with the top of the tubular reactor 4, the other end of the outer cannula 5 is communicated with the gas-liquid separation tank 6, one end of the transportation component 7 penetrates through the bottom of the tubular reactor 4, the other end of the conveying component 7 is respectively communicated with the bottom of the first secondary acidolysis kettle 9 and the bottom of the second secondary acidolysis kettle 10, the control component 8 penetrates through the conveying component 7, one end of the air inlet pipe 11 is communicated with the gas-liquid separation tank 6, the other end of the air inlet pipe 11 is respectively communicated with the first secondary acidolysis kettle 9 and the second secondary acidolysis kettle 10, the absorption component 12 is communicated with the gas-liquid separation tank 6, one end of the gas circulation pipe 13 is communicated with the gas storage tank 2, the other end of the gas circulation pipe 13 is respectively communicated with the first secondary acidolysis kettle 9 and the second secondary acidolysis kettle 10, the first valve 15 penetrates through the outer side wall of the gas circulation pipe 13 and is close to the first secondary acidolysis kettle 9, and the second valve 16 penetrates through the outer side wall of the gas circulation pipe 13, and is close to the second-stage acidolysis kettle 10.

In the present embodiment, when a technician uses 2-chloroethylphosphonic acid bis- (2-chloroethyl) ester to produce ethephon, 2-chloroethylphosphonic acid bis- (2-chloroethyl) ester is placed in the material storage tank 1, hydrogen chloride gas is placed in the gas storage tank 2, and the transport means 3 causes the 2-chloroethylphosphonic acid bis- (2-chloroethyl) ester and the hydrogen chloride gas to flow downstream into the tubular reactor 4 from the bottom of the tubular reactor 4 and react with each other, respectively, so that the molar ratio of hydrogen chloride to 2-chloroethylphosphonic acid bis- (2-chloroethyl) ester is 2 to 2.5: 1, reducing the consumption of raw materials and reducing the amount of tail gas and byproducts, controlling the pressure in the tubular reactor 4 at 0.1-0.5MPa and the temperature at 120-200 ℃, and extracting the excessive tail gas and byproduct dichloroethane from the top of the tubular reactor 4 to the gas-liquid separation tank 6; meanwhile, the reaction mixed liquid of the 2-chloroethyl di- (2-chloroethyl) phosphonate and the hydrogen chloride gas in the tubular reactor 4 respectively enters the first secondary acidolysis kettle 9 and the second secondary acidolysis kettle 10 through the conveying component 7, the first air pump 14 is controlled, the third valve 81 and the fourth valve 82 are adjusted according to the working states of the first secondary acidolysis kettle 9 and the second secondary acidolysis kettle 10, fresh hydrogen chloride gas is injected into the first secondary acidolysis kettle 9 and the second secondary acidolysis kettle 10, the pressure in the first secondary acidolysis kettle 9 and the pressure in the second secondary acidolysis kettle 10 are both controlled to be 0.1-0.5MPa, the temperature is both controlled to be 120-phase-200 ℃, the excessive hydrogen chloride gas and the byproduct dichloroethane in the first secondary acidolysis kettle 9 and the second secondary acidolysis kettle 10 and the tail gas and the byproduct dichloroethane generated in the tubular reactor 4 enter the gas together The liquid separation tank 6 is used for gas-liquid separation, and the gas absorption component 12 is used for absorption treatment, so that the technical personnel can conveniently treat the tail gas and byproduct dichloroethane gas generated in the production of ethephon.

Further, the transportation assembly 3 includes a first transportation pipe 31 and a transfer pump 32, one end of the first transportation pipe 31 is communicated with the material storage tank 1, the other end of the first transportation pipe 31 is communicated with the bottom of the tubular reactor 4, and the transfer pump 32 penetrates through the outer side wall of the first transportation pipe 31.

Further, the transportation assembly 3 further includes a second transportation pipe 33 and a second air pump 34, one end of the second transportation pipe 33 is communicated with the gas storage tank 2, the other end of the second transportation pipe 33 is communicated with the first transportation pipe 31, and the second air pump 34 penetrates through the outer side wall of the second transportation pipe 33.

In this embodiment, when a technician produces ethephon from 2-chloroethylphosphonic acid bis- (2-chloroethyl) ester, 2-chloroethylphosphonic acid di- (2-chloroethyl) ester is placed in the material storage tank 1, hydrogen chloride gas is placed in the gas storage tank 2, the operation of the material transfer pump 32 is controlled, so that the bis- (2-chloroethyl) 2-chloroethylphosphonate in the material storage tank 1 flows co-currently from the bottom of the tubular reactor 4 to the tubular reactor 4 via the first transport pipe 31, and simultaneously controlling the second water pump so that the hydrogen chloride gas in the gas storage tank 2 flows downstream from the bottom of the tubular reactor 4 to the tubular reactor 4 through the second transport pipe 33, and the molar ratio of hydrogen chloride to bis- (2-chloroethyl) 2-chloroethylphosphonate is 2-2.5: 1, the raw material consumption is reduced, and the amount of tail gas and byproducts is reduced.

Further, the control assembly 8 comprises a third valve 81 and a fourth valve 82, and the third valve 81 and the fourth valve 82 respectively extend through the delivery assembly 7.

In this embodiment, when a technician starts to produce ethephon, the technician opens the third valve 81 and the first valve 15, closes the fourth valve 82 and the third valve 81, and the reacted mixture enters the first secondary acidolysis vessel 9 through the delivery module 7, and starts the first air pump 14 to inject fresh hydrogen chloride gas into the first secondary acidolysis vessel 9; after one kilogram of reaction mixed liquid is collected, the third valve 81 and the first valve 15 are closed, the fourth valve 82 is opened, the third valve 81 is opened, the reacted mixed liquid enters the second-stage acidolysis kettle 10 through the conveying assembly 7, the first air pump 14 is started, and fresh hydrogen chloride gas is injected into the second-stage acidolysis kettle 10.

Further, the conveying assembly 7 comprises an inner insertion pipe 71, a first branch pipe 72 and a second branch pipe 73, one end of the inner insertion pipe 71 penetrates through the bottom of the tubular reactor 4, the other end of the inner insertion pipe 71 is communicated with the first branch pipe 72 and the second branch pipe 73 respectively, the first branch pipe 72 is communicated with the bottom of the first secondary acid hydrolysis kettle 9, the second branch pipe 73 is communicated with the bottom of the second secondary acid hydrolysis kettle 10, the third valve 81 penetrates through the outer side wall of the first branch pipe 72, and the fourth valve 82 penetrates through the outer side wall of the second branch pipe 73.

In this embodiment, one end of the inner pipe 71 is located in the tubular reactor 4, and the reaction mixture of bis- (2-chloroethyl) 2-chloroethylphosphonate and hydrogen chloride passes through the inner pipe 71, and enters the first secondary acid hydrolysis reactor 9 from the first branch pipe 72 and enters the second secondary acid hydrolysis reactor 10 from the second branch pipe 73, respectively.

Further, the absorption assembly 12 comprises an exhaust pipe 19 and a tail gas absorption kettle 20, wherein one end of the exhaust pipe 19 is communicated with the gas-liquid separation tank 6, and the other end of the exhaust pipe 19 is communicated with the tail gas absorption kettle 20.

In the present embodiment, the gas-liquid separation tank 6 contains the off-gas and by-product dichloroethane generated from the tubular reactor 4 and the excess hydrogen chloride in the first secondary acid hydrolysis reactor 9 and the second secondary acid hydrolysis reactor 10, and a technician discharges the gas in the gas-liquid separation tank 6 to the off-gas absorption reactor 20 through the exhaust pipe 19 to perform collection treatment.

Further, the tubular reactor 4 includes a column 41, a connection cover 42, glass filler 43, a filler placing rack 44 and abutting components 45, the connection cover 42 is fixedly connected with the column 41 and is located above the column 41, one end of the outer cannula 5 is communicated with the connection cover 42, the glass filler 43 is detachably connected with the filler placing rack 44, the column 41 is provided with an installation groove 17, the filler placing rack 44 is detachably connected with the column 41, two sides of the filler placing rack 44 are embedded in the installation groove 17, the filler placing rack 44 is provided with two abutting grooves 18, the number of the abutting components 45 is two, and each group of the abutting components 45 is located in the installation groove 17 and is in contact with the corresponding abutting groove 18;

each group of the abutting assemblies 45 respectively comprises an extension spring 47, an abutting block 48 and a pulling strip 49, one end of the extension spring 47 is fixedly connected with the cylinder 41 and is positioned in the mounting groove 17, the other end of the extension spring 47 is fixedly connected with the abutting block 48, the abutting block 48 is matched with the abutting groove 18, the pulling strip 49 is fixedly connected with the abutting block 48 and is close to the extension spring 47, and one end of the pulling strip 49 penetrates through the outer side wall of the cylinder 41.

In this embodiment, the length of the tubular reactor is 50cm, the inner diameter is 85mm, when a technician needs to replace a new glass filler 43, the technician holds the two pulling strips 49 with hands, the two abutting blocks 48 abut against the corresponding abutting grooves 18 respectively at this time, so that the filler placing frame 44 is fixed relative to the column 41, the technician pulls the pulling strips 49, the abutting blocks 48 pull down the pulling strips 49, so that the extension springs 47 are compressed, the abutting blocks 48 leave the abutting grooves 18 at this time, the filler placing frame 44 is loosened, the technician holds the lower side of the filler placing frame 44, takes down the filler placing frame 44, and replaces the new glass filler 43; after the replacement is finished, the technician holds the filler placing frame 44, aligns the edge of the side wall of the filler placing frame 44 in the mounting groove 17, and pulls the pulling strip 49, so that the outer side wall of the filler placing frame 44 abuts against the abutting block 48, at the moment, the pulling strip 49 is loosened, the filler placing frame 44 is pushed, the abutting block 48 is located at the abutting groove 18, at the moment, under the action of the resilience force of the extension spring 47, the abutting block 48 enters the abutting groove 18, so that the filler placing frame 44 is fixed relative to the column 41, and the replacement of the glass filler 43 by the technician is facilitated.

Further, the tubular reactor 4 further comprises a sealing strip 46, wherein the sealing strip 46 is fixedly connected with the column 41 and surrounds the connection position of the column 41 and the filler placing frame 44.

In this embodiment, the sealing strip 46 surrounds the connection between the column 41 and the filler placing frame 44, and the sealing strip 46 plays a role of sealing to prevent the reaction mixture from permeating out from the connection between the column 41 and the filler placing frame 44 when the tubular reactor 4 is in operation.

Referring to fig. 1, the present invention further provides a continuous production method of ethephon by using the above continuous production apparatus of ethephon, comprising the following steps:

s1: starting the transfer pump 32 to transport 2-chloroethylphosphonic acid bis- (2-chloroethyl) ester from the material storage tank 1 through the first transport pipe 31 into the tubular reactor 4;

s2: starting the second air pump 34, conveying fresh hydrogen chloride gas from the gas storage tank 2 into the tubular reactor 4 through the second conveying pipe 33, and continuously reacting with 2-chloroethylphosphonic acid di- (2-chloroethyl) ester;

s3: opening the third valve 81 and the first valve 15, closing the fourth valve 82 and the third valve 81, allowing the reacted mixture to enter the first secondary acidolysis kettle 9 through the inner insertion tube 71, starting the first air pump 14, and injecting fresh hydrogen chloride gas into the first secondary acidolysis kettle 9;

s4: after one kilogram of mixed liquid is collected, the third valve 81 and the first valve 15 are closed, the fourth valve 82 and the third valve 81 are opened, the mixed liquid after reaction enters the second-stage acidolysis kettle 10 through the inner insertion pipe 71, the first air pump 14 is started, and fresh hydrogen chloride gas is injected into the second-stage acidolysis kettle 10;

s5: separating the tail gas and by-product dichloroethane generated from the tubular reactor 4 and the excess hydrogen chloride in the first secondary acid hydrolysis kettle 9 and the second secondary acid hydrolysis kettle 10 in the gas-liquid separation tank 6;

s6: and discharging the gas in the gas-liquid separation tank 6 to the tail gas absorption kettle 20 through the exhaust pipe 19 for collection.

Wherein, the material transferring pump 32 is started first, the 2-chloroethyl phosphonic acid bis- (2-chloroethyl) ester is transported from the material storage tank 1 to the tubular reactor 4 through the first transport pipe 31, the flow rate of the 2-chloroethyl phosphonic acid bis- (2-chloroethyl) ester is 160g/h, the second air pump 34 is started, the fresh hydrogen chloride gas is transported from the gas storage tank 2 to the tubular reactor 4 through the second transport pipe 33, the flow rate of the hydrogen chloride gas is 460mL/min, the reaction pressure of the hydrogen chloride gas and the 2-chloroethyl phosphonic acid bis- (2-chloroethyl) ester in the tubular reactor 4 is 0.2MPa, the temperature is 145-150 ℃, the residence time is 8h, and then the third valve 81 and the first valve 15 are opened, closing the fourth valve 82 and the third valve 81, allowing the reacted mixture to enter the first secondary acidolysis kettle 9 through the inner insertion tube 71, starting the first air pump 14, injecting fresh hydrogen chloride gas into the first secondary acidolysis kettle 9, allowing the hydrogen chloride gas to flow at a flow rate of 200mL/min and a reaction pressure of 0.2MPa and a temperature of 145- And finally, discharging the gas in the gas-liquid separation tank 6 to the tail gas absorption kettle 20 through the exhaust pipe 19 for collection, wherein the analysis result shows that the purity of the produced ethephon is 95.6 percent, and the 2-chloroethylphosphonic acid anhydride is less than 0.1 percent.

While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

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