CN110150268B - Preparation process for continuously producing ethephon aqua - Google Patents
Preparation process for continuously producing ethephon aqua Download PDFInfo
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- CN110150268B CN110150268B CN201910434896.7A CN201910434896A CN110150268B CN 110150268 B CN110150268 B CN 110150268B CN 201910434896 A CN201910434896 A CN 201910434896A CN 110150268 B CN110150268 B CN 110150268B
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- UDPGUMQDCGORJQ-UHFFFAOYSA-N (2-chloroethyl)phosphonic acid Chemical compound OP(O)(=O)CCCl UDPGUMQDCGORJQ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000005976 Ethephon Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims description 23
- 238000003756 stirring Methods 0.000 claims abstract description 122
- 238000004140 cleaning Methods 0.000 claims abstract description 48
- 239000002994 raw material Substances 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- -1 diester phosphate Chemical class 0.000 claims abstract description 30
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 27
- 239000010452 phosphate Substances 0.000 claims abstract description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 12
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 12
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000007789 sealing Methods 0.000 claims description 56
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 21
- 239000000460 chlorine Substances 0.000 claims description 21
- 229910052801 chlorine Inorganic materials 0.000 claims description 21
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000003814 drug Substances 0.000 claims description 14
- 238000003556 assay Methods 0.000 claims description 12
- 238000005070 sampling Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 7
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims description 7
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000010924 continuous production Methods 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- 150000005691 triesters Chemical class 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/12—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing acyclic or cycloaliphatic radicals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0073—Sealings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/28—Moving reactors, e.g. rotary drums
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Plant Pathology (AREA)
- Agronomy & Crop Science (AREA)
- Toxicology (AREA)
- Mixers Of The Rotary Stirring Type (AREA)
- Management, Administration, Business Operations System, And Electronic Commerce (AREA)
Abstract
The invention discloses a ethephon aqua which comprises the following raw materials in parts by weight, 80-100 parts of diester phosphate, 10-30 parts of hydrogen chloride gas and 30-50 parts of water; inside pouring into the staving with the feed inlet of diester phosphate from agitating unit, heat the staving, the cleaning brush wholly carries out abundant cleaning work to the inner wall of staving, clean the completion back, move to the inboard of stirring the leaf through second pneumatic cylinder control second piston push rod, make the inside of cleaning brush retraction rectangular channel, the spring exerts elasticity to the baffle, make the closing plate remove downwards, plug up the notch of rectangular channel, avoid the raw materials to get into, can both carry out staving inner wall cleaning work after every stirring is accomplished, guarantee the raw materials allotment precision, do not need the manual washing of workman, save physical power, and guarantee that the staving inner wall can wholly clean, improve clean effect.
Description
Technical Field
The invention relates to the field of ethephon preparation, in particular to a preparation process for continuously producing ethephon water aqua.
Background
The chemical name of ethephon is 2-chloroethylphosphonic acid, the ethephon has good water solubility, is used on crops, usually adopts water aqua, and currently, 40 percent of ethephon water aqua is widely used. In order to reduce the packaging and transportation cost and improve the use effect, manufacturers try to improve the concentration of the ethephon water aqua.
At present, the preparation of the ethephon aqua regia needs to use the diester phosphate, but in the preparation process of the diester phosphate, sufficient ethylene oxide needs to be blended into phosphorus trichloride at one time, the mass fraction of free chlorine is detected, so that the phosphorus trichloride is wasted, and in the preparation of the ethephon aqua regia, a container processed at the last time needs to be cleaned when continuous processing is needed, and the container needs to be cleaned manually or cleaned by using a water gun at present, so that the cleaning is incomplete, the blending precision is influenced, and the cleaning is difficult.
Disclosure of Invention
The invention aims to provide a preparation process for continuously producing a ethephon aqua, which aims to solve the problems that the existing ethephon aqua preparation needs to use diester phosphate, but in the preparation process of the diester phosphate, phosphorus trichloride needs to be blended with sufficient ethylene oxide at one time, and then the mass fraction of free chlorine is detected, so that the phosphorus trichloride is wasted, and in the preparation of the ethephon aqua, a container processed last time needs to be cleaned when continuous processing is needed, and the existing cleaning container needs to be cleaned manually or by a water gun, so that the cleaning is incomplete, the blending precision is influenced, and the cleaning is difficult.
The purpose of the invention can be realized by the following technical scheme:
the ethephon water aqua comprises the following raw materials in parts by weight:
80-100 parts of diester phosphate, 10-30 parts of hydrogen chloride gas and 30-50 parts of water;
the phosphoric acid diester is prepared by the following steps:
the method comprises the following steps: adding 500g of phosphorus trichloride into a reaction kettle in an environment of-5 ℃, introducing ethylene oxide into the reaction kettle, keeping the temperature at 30 ℃, stirring for 3 hours, sampling for assay, taking materials when free chlorine reaches 0.1-0.3mg/kg, continuing to introduce ethylene oxide, sampling for assay after stirring for 30 minutes, taking materials when free chlorine reaches 0.1-0.3mg/kg, and repeating the operation until the free chlorine reaches 0.1-0.3 mg/kg;
step two: adding the product in the step one to the temperature of 240 ℃ to 250 ℃, and stirring for 20 minutes to obtain the diester phosphate;
the ethephon water aqua is prepared by the following preparation process:
inside injecting into the staving with the diester phosphate from the charge door in agitating unit, heat the staving, make it reach 175 ℃, the discharge gate lets in the hydrogen chloride gas, make its abundant reaction, until dichloroethane is not in the formation, stop ventilating, the inside injected water of rethread dosing mouth to the staving, the output of motor passes through shaft coupling drive (mixing) shaft and takes place to rotate, when the (mixing) shaft rotates, drive the stirring leaf of its bottom and rotate, stir the work to the inside raw materials of staving, reciprocate through the inside first piston push rod of first pneumatic cylinder controller, make the bung wholly reciprocate, make the whole stirring that all stirs of raw materials, make the stirring more even, after the stirring is accomplished, the ethylene water aqua that produces is discharged through the discharge gate of staving bottom, accomplish the preparation work to the ethylene water aqua.
As a further scheme of the invention: in the preparation process of the diester phosphate, ethylene oxide is introduced into a reaction kettle, the temperature is kept at 30 ℃, stirring is carried out, sampling is carried out for assay after stirring is carried out for 3 hours, the material can be taken when the free chlorine reaches 0.1-0.3mg/kg, the ethylene oxide is introduced again if not, sampling is carried out for assay after stirring is carried out for 30 minutes, the material can be taken when the free chlorine reaches 0.1-0.3mg/kg, otherwise, the operation is repeated until the free chlorine reaches 0.1-0.3mg/kg, and compared with the traditional method of directly introducing sufficient ethylene oxide, the dosage of the ethylene oxide can be saved.
As a further scheme of the invention: in the preparation process of the diester phosphate, the reaction temperature is 240-250 ℃, and then stirring treatment is carried out for 20 minutes, so that the triester phosphite is used for generating the diester phosphate, and the reaction is ensured to be more thorough.
A preparation process of a ethephon aqua specifically comprises the following steps:
s1, injecting the diester phosphate into the barrel body from the interior of a feed inlet in the stirring device, heating the barrel body to 175 ℃, introducing hydrogen chloride gas into a discharge outlet to fully react until dichloroethane is not generated, and stopping introducing the hydrogen chloride gas;
s2, injecting water into the barrel through the medicine adding port, driving the stirring shaft to rotate through the coupler by the output end of the motor, driving the stirring blades at the bottom of the stirring shaft to rotate when the stirring shaft rotates, stirring the raw materials in the barrel, and moving the barrel cover up and down through the first piston push rod in the first hydraulic cylinder controller so that the whole barrel cover moves up and down, so that the whole raw materials are stirred uniformly, and after stirring is finished, discharging the generated ethephon aqua through the discharge port at the bottom end of the barrel;
s3, when the ethephon aqua is continuously produced, the inner wall of the barrel body needs to be cleaned, a second piston push rod is controlled by a second hydraulic cylinder to move towards the outer side of the stirring blade, the second piston push rod applies pressure to the sealing plate, the sealing plate moves towards the inside of the sealing groove due to the fact that the side wall of the sealing plate is an inclined wall, the baffle applies pressure to the spring, the spring is compressed, the second piston push rod extends out of the outer side of the stirring blade, a cleaning brush at one end of the second piston push rod is in contact with the inner wall of the barrel body and moves up and down through a first piston push rod in a first hydraulic cylinder controller, the whole barrel cover moves up and down, meanwhile, clear water is added from a dosing port and a feeding port, and the cleaning brush fully cleans the whole inner wall of the barrel body;
s4, after cleaning, controlling the second piston push rod to move towards the inner side of the stirring blade through the second hydraulic cylinder, enabling the cleaning brush to retract into the rectangular groove, applying elasticity to the baffle plate through the spring, enabling the sealing plate to move downwards to block the notch of the rectangular groove, preventing raw materials from entering, adding the diester phosphate and other raw materials again, and achieving continuous production of the ethylene aqua.
As a further scheme of the invention: the stirring device comprises a base, a barrel body and a sealing plate, wherein the top of the base is fixedly provided with the barrel body, the bottom of the barrel body is provided with a discharge port, the outer surface of the barrel body is provided with a reinforcing plate, the top surface of the base around the barrel body is respectively provided with four first hydraulic cylinders, first piston push rods are arranged inside the four first hydraulic cylinders, the top position of the side wall of the barrel body is provided with a lower end cover, a barrel cover is arranged above the barrel body, the bottom of the side wall of the barrel cover is provided with an upper end cover at a position corresponding to the lower end cover, a sealing rubber strip is arranged between the upper end cover and the lower end cover, a mounting frame is welded at the middle position of the top surface of the barrel cover, one side of the mounting frame is provided with a feed inlet, the other side of the mounting frame is provided with a medicine feeding port, the top of the feed inlet is provided with a sealing cover, a handle is arranged on the sealing cover, the side wall of the barrel cover is welded with four transverse shafts, and the top ends of the four first piston push rods are fixedly connected with the bottom surfaces of the transverse shafts, a motor is fixedly installed at the top of the mounting frame, a stirring shaft is arranged at the bottom of the motor, the output end of the motor is in transmission connection with the top end of the stirring shaft through a coupler, the bottom end of the stirring shaft penetrates through the barrel cover and extends into the barrel body, stirring blades are arranged at the bottom end of the stirring shaft, rectangular grooves are formed in the two end structures of the stirring blades, a second hydraulic cylinder is respectively arranged in each of the two rectangular grooves, a second piston push rod is arranged in each second hydraulic cylinder, one end of each second piston push rod penetrates through the inner wall of the second hydraulic cylinder, a cleaning brush is arranged on the end face of each second piston push rod, a sealing groove is formed in each stirring blade above the cleaning brush, a baffle is arranged in each sealing groove, a sealing plate is fixedly connected to one side of each baffle, the side wall of each sealing plate, which is adjacent to the cleaning brush, is an inclined wall, a spring is arranged between the other side of each baffle and the inner wall of each sealing groove, and when the sealing cover is opened through a handle, the raw material is injected from the interior of the feed inlet, another raw material is injected into the interior of the barrel body through the drug adding port, the output end of the motor drives the stirring shaft to rotate through the coupler, when the stirring shaft rotates, the stirring blade at the bottom of the stirring shaft is driven to rotate, the raw material in the barrel body is stirred, the first piston push rod in the first hydraulic cylinder controller moves up and down, so that the whole barrel cover moves up and down, the whole raw material is stirred uniformly, after the stirring is finished, the raw material is discharged through the discharge port at the bottom end of the barrel body, when the raw material needs to be stirred again, the inner wall of the barrel body needs to be cleaned, the second piston push rod is controlled by the second hydraulic cylinder to move towards the outer side of the stirring blade, the second piston push rod applies pressure to the sealing plate, because the side wall of the sealing plate is an inclined wall, the sealing plate moves towards the interior of the sealing groove, and the baffle applies pressure to the spring, the spring is compressed, the second piston push rod extends out of the outer side of the stirring blade, the cleaning brush at one end of the second piston push rod is in contact with the inner wall of the barrel body, the first piston push rod in the first hydraulic cylinder controller moves up and down to enable the barrel cover to integrally move up and down, clean water is added from the medicine feeding port and the material feeding port at the same time, the cleaning brush fully cleans the whole inner wall of the barrel body, after cleaning is completed, the second piston push rod is controlled by the second hydraulic cylinder to move towards the inner side of the stirring blade, so that the cleaning brush retracts into the rectangular groove, the spring exerts elastic force on the baffle plate, the sealing plate moves downwards to block the notch of the rectangular groove to avoid raw material entering, cleaning work on the inner wall of the barrel body can be performed after each stirring is completed, raw material blending precision is ensured, manual cleaning by workers is not needed, physical strength is saved, and the inner wall of the barrel body can be integrally cleaned, the cleaning effect is improved.
The invention has the beneficial effects that:
1. in the preparation process of the diester phosphate, the ethylene oxide is introduced into a reaction kettle, the temperature is kept at 30 ℃, stirring is carried out, sampling is carried out for assay after stirring is carried out for 3 hours, the material can be taken when the free chlorine reaches 0.1-0.3mg/kg, the ethylene oxide is introduced again if not, sampling is carried out for assay after stirring is carried out for 30 minutes, the material can be taken when the free chlorine reaches 0.1-0.3mg/kg, otherwise, the operation is repeated until the free chlorine reaches 0.1-0.3mg/kg, and compared with the traditional method of directly introducing sufficient ethylene oxide, the dosage of the ethylene oxide can be saved;
2. in the invention, the output end of a motor drives a stirring shaft to rotate through a coupler, when the stirring shaft rotates, stirring blades at the bottom of the stirring shaft are driven to rotate, raw materials in a barrel body are stirred, a first piston push rod in a first hydraulic cylinder controller moves up and down to enable the barrel cover to move up and down integrally, so that the raw materials are stirred uniformly, after the stirring is completed, the raw materials are discharged through a discharge port at the bottom end of the barrel body, when the raw materials are required to be stirred again, the inner wall of the barrel body needs to be cleaned, a second piston push rod is controlled by a second hydraulic cylinder to move to the outer side of the stirring blades, the second piston push rod applies pressure to a sealing plate, as the side wall of the sealing plate is an inclined wall, the sealing plate moves to the inside of a sealing groove, a baffle applies pressure to a spring, so that the spring is compressed, and the second piston push rod extends out of the stirring blades, the cleaning brush of second piston push rod one end contacts with the inner wall of staving, it reciprocates through the inside first piston push rod of first pneumatic cylinder controller, make the bung wholly reciprocate, add the clear water from medicine feed inlet and charge door simultaneously, the cleaning brush wholly carries out abundant cleaning work to the inner wall of staving, clean the completion back, move to the inboard of stirring the leaf through second pneumatic cylinder control second piston push rod, make the cleaning brush retract the inside of rectangular channel, the spring exerts elasticity to the baffle, make the closing plate downstream, plug up the notch of rectangular channel, avoid the raw materials to get into, can both carry out staving inner wall cleaning work after stirring is accomplished at every turn, guarantee raw materials allotment precision, do not need workman manual washing, save physical power, and guarantee that the staving inner wall can wholly clean, improve clean effect.
Drawings
In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic view of a stirring apparatus according to the present invention;
FIG. 2 is a top view of the stirring device of the present invention;
FIG. 3 is a partial enlarged view A of the present invention;
FIG. 4 is a partial enlarged view B of the present invention;
in the figure: 1. a base; 2. stirring blades; 3. a reinforcing plate; 4. a first hydraulic cylinder; 5. a first piston pushrod; 6. a horizontal axis; 7. a medicine adding port; 8. a mounting frame; 9. a motor; 10. sealing the cover; 11. a handle; 12. a feed inlet; 13. a barrel cover; 14. a stirring shaft; 15. a barrel body; 16. a second hydraulic cylinder; 17. a discharge port; 18. an upper end cover; 19. a lower end cover; 20. a spring; 21. a sealing groove; 22. a baffle plate; 23. a sealing plate; 24. a cleaning brush; 25. a second piston push rod; 26. a rectangular groove.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1-4, the ethephon water aqua comprises the following raw materials in parts by weight:
80-100 parts of diester phosphate, 10-30 parts of hydrogen chloride gas and 30-50 parts of water;
the phosphoric acid diester is prepared by the following steps:
the method comprises the following steps: adding 500g of phosphorus trichloride into a reaction kettle in an environment of-5 ℃, introducing ethylene oxide into the reaction kettle, keeping the temperature at 30 ℃, stirring for 3 hours, sampling for assay, taking materials when free chlorine reaches 0.1-0.3mg/kg, continuing to introduce ethylene oxide, sampling for assay after stirring for 30 minutes, taking materials when free chlorine reaches 0.1-0.3mg/kg, and repeating the operation until the free chlorine reaches 0.1-0.3 mg/kg;
step two: adding the product in the step one to the temperature of 240 ℃ to 250 ℃, and stirring for 20 minutes to obtain the diester phosphate;
the ethephon water aqua is prepared by the following preparation process:
the diester phosphate is injected into the barrel body 15 from the interior of a feed inlet 12 in the stirring device, the barrel body 15 is heated to 175 ℃, hydrogen chloride gas is introduced into a discharge outlet 17 to fully react until dichloroethane is not generated, the ventilation is stopped, water is injected into the barrel body 15 through a drug adding port 7, the output end of a motor 9 drives a stirring shaft 14 to rotate through a coupler, and when the stirring shaft 14 rotates, a stirring blade 2 at the bottom of the stirring shaft is driven to rotate, the raw materials in the barrel body 15 are stirred and move up and down through a first piston push rod 5 in the first hydraulic cylinder 4 controller, the barrel cover 13 is integrally moved up and down, so that the raw materials are integrally stirred, the stirring is more uniform, after the stirring is finished, the generated ethephon water agent is discharged through a discharge hole 17 at the bottom end of the barrel body 15, and the preparation work of the ethephon water agent is completed.
In the preparation process of the diester phosphate, introducing ethylene oxide into a reaction kettle, keeping the temperature at 30 ℃, stirring for 3 hours, sampling for assay, taking materials when the free chlorine reaches 0.1-0.3mg/kg, and continuing to introduce ethylene oxide if the free chlorine does not reach 0.1-0.3mg/kg, and sampling for assay after stirring for 30 minutes, wherein the materials can be taken when the free chlorine reaches 0.1-0.3mg/kg, otherwise, repeating the operation until the free chlorine reaches 0.1-0.3mg/kg, and compared with the traditional method of directly introducing sufficient ethylene oxide, the method can save the dosage of the ethylene oxide.
In the preparation process of the diester phosphate, the reaction temperature is 240-250 ℃, and then stirring treatment is carried out for 20 minutes, so that the triester phosphite is generated into the diester phosphate, and the reaction is ensured to be more thorough.
A preparation process of a ethephon aqua specifically comprises the following steps:
s1, injecting the diester phosphate into the barrel body 15 from the interior of the feed inlet 12 in the stirring device, heating the barrel body 15 to 175 ℃, introducing hydrogen chloride gas into the discharge outlet 17 to fully react until dichloroethane is not generated, and stopping introducing the hydrogen chloride gas;
s2, injecting water into the barrel body 15 through the medicine adding port 7, driving the stirring shaft 14 to rotate through the coupler by the output end of the motor 9, driving the stirring blades 2 at the bottom of the stirring shaft 14 to rotate when the stirring shaft 14 rotates, stirring the raw materials in the barrel body 15, and moving the barrel cover 13 up and down through the first piston push rod 5 in the first hydraulic cylinder 4 controller, so that the whole barrel cover 13 is moved up and down, the raw materials are stirred uniformly, and the generated ethylene aqua-aquae is discharged through the discharge port 17 at the bottom end of the barrel body 15 after stirring;
s3, when the ethephon aqua agent is continuously produced, the inner wall of a barrel body 15 needs to be cleaned, a second piston push rod 25 is controlled to move towards the outer side of a stirring blade 2 through a second hydraulic cylinder 16, the second piston push rod 25 applies pressure to a sealing plate 23, the sealing plate 23 moves towards the inside of a sealing groove 21 due to the fact that the side wall of the sealing plate 23 is an inclined wall, a baffle plate 22 applies pressure to a spring 20 to compress the spring 20, the second piston push rod 25 extends out of the stirring blade 2, a cleaning brush 24 at one end of the second piston push rod 25 is in contact with the inner wall of the barrel body 15, the first piston push rod 5 in the first hydraulic cylinder 4 is controlled to move up and down, the barrel cover 13 integrally moves up and down, meanwhile, clear water is added from a dosing port 7 and a dosing port 12, and the cleaning brush 24 fully cleans the inner wall of the barrel body 15;
s4, after cleaning, controlling the second piston push rod 25 to move towards the inner side of the stirring blade 2 through the second hydraulic cylinder 16, enabling the cleaning brush 24 to retract into the rectangular groove 26, applying elastic force to the baffle 22 through the spring 20, enabling the sealing plate 23 to move downwards, blocking the notch of the rectangular groove 26, avoiding raw materials from entering, adding diester phosphate and other raw materials again, and realizing continuous production of the ethephon aqua.
The stirring device comprises a base 1, a barrel body 15 and a sealing plate 23, wherein the top of the base 1 is fixedly provided with the barrel body 15, the bottom of the barrel body 15 is provided with a discharge hole 17, the outer surface of the barrel body 15 is provided with a reinforcing plate 3, the top surface of the base 1 around the barrel body 15 is respectively provided with four first hydraulic cylinders 4, the insides of the four first hydraulic cylinders 4 are provided with first piston push rods 5, the top position of the side wall of the barrel body 15 is provided with a lower end cover 19, a barrel cover 13 is arranged above the barrel body 15, the bottom of the side wall of the barrel cover 13 is provided with an upper end cover 18 at a position corresponding to the lower end cover 19, a sealing rubber strip is arranged between the upper end cover 18 and the lower end cover 19, the middle position of the top surface of the barrel cover 13 is welded with a mounting frame 8, one side of the mounting frame 8 is provided with a feed inlet 12, the other side of the mounting frame 8 is provided with a medicine feeding port 7, the top of the feed inlet 12 is provided with a sealing cover 10, the sealing cover 10 is provided with a handle 11, the side wall of the barrel cover 13 is welded with four cross shafts 6, the top ends of four first piston push rods 5 are fixedly connected with the bottom surface of a cross shaft 6, the top of a mounting frame 8 is fixedly provided with a motor 9, the bottom of the motor 9 is provided with a stirring shaft 14, the output end of the motor 9 is in transmission connection with the top end of the stirring shaft 14 through a coupler, the bottom end of the stirring shaft 14 penetrates through a barrel cover 13 and extends into a barrel body 15, the bottom end of the stirring shaft 14 is provided with a stirring blade 2, two end structures of the stirring blade 2 are internally provided with rectangular grooves 26, two rectangular grooves 26 are internally provided with second hydraulic cylinders 16 respectively, a second piston push rod 25 is arranged inside the second hydraulic cylinders 16, one end of the second piston push rod 25 penetrates through the inner wall of the second hydraulic cylinders 16, the end surface of the second piston push rod 25 is provided with a cleaning brush 24, the inside of the stirring blade 2 above the cleaning brush 24 is provided with a sealing groove 21, the inside of the sealing groove 21 is provided with a baffle 22, and one side of the baffle 22 is fixedly connected with a sealing plate 23, the side wall of one side of the sealing plate 23 adjacent to the cleaning brush 24 is an inclined wall, a spring 20 is arranged between the other side of the baffle 22 and the inner wall of the sealing groove 21, when the device is used, the sealing cover 10 is opened through the handle 11, raw materials are injected from the inside of the feed inlet 12, another raw material is injected into the barrel body 15 through the drug adding port 7, the output end of the motor 9 drives the stirring shaft 14 to rotate through the coupler, the stirring blade 2 at the bottom of the stirring shaft 14 is driven to rotate when the stirring shaft 14 rotates, the raw materials in the barrel body 15 are stirred, the barrel cover 13 is driven to move up and down through the first piston push rod 5 in the first hydraulic cylinder 4 controller, the whole barrel cover 13 is stirred, the whole raw materials are stirred uniformly, after the stirring is completed, the raw materials are discharged through the discharge port 17 at the bottom of the barrel body 15, when the raw materials are required to be stirred again, the inner wall of the barrel body 15 needs to be cleaned, the second piston push rod 25 is controlled to move towards the outer side of the stirring blade 2 through the second hydraulic cylinder 16, the second piston push rod 25 applies pressure to the sealing plate 23, the sealing plate 23 moves towards the inside of the sealing groove 21 due to the fact that the side wall of the sealing plate 23 is an inclined wall, the baffle plate 22 applies pressure to the spring 20, the spring 20 is compressed, the second piston push rod 25 extends out of the outer side of the stirring blade 2, the cleaning brush 24 at one end of the second piston push rod 25 is in contact with the inner wall of the barrel body 15, the first piston push rod 5 in the first hydraulic cylinder 4 controller moves up and down, the barrel cover 13 moves up and down integrally, meanwhile, clear water is added from the medicine adding opening 7 and the material adding opening 12, the cleaning brush 24 fully cleans the inner wall of the barrel body 15, after cleaning is completed, the second piston push rod 25 is controlled to move towards the inner side of the stirring blade 2 through the second hydraulic cylinder 16, and, spring 20 exerts elasticity to baffle 22 for closing plate 23 moves down, plugs up the notch of rectangular channel 26, avoids the raw materials to get into, can both carry out staving 15 inner wall cleaning work after stirring is accomplished at every turn, guarantees the raw materials allotment precision, does not need workman manual washing, saves physical power, and guarantees that staving 15 inner walls can wholly clean, improves clean effect.
The working principle of the invention is as follows: injecting diester phosphate into a barrel body 15 from the inside of a feed inlet 12 in a stirring device, heating the barrel body 15 to 175 ℃, introducing hydrogen chloride gas into a discharge outlet 17 to fully react until dichloroethane is not generated, and stopping ventilation, injecting water into the barrel body 15 through a drug adding port 7, driving a stirring shaft 14 to rotate by an output end of a motor 9 through a coupler, driving a stirring blade 2 at the bottom of the stirring shaft 14 to rotate when the stirring shaft 14 rotates, stirring the raw material in the barrel body 15, controlling a first piston push rod 5 in a controller to move up and down through a first hydraulic cylinder 4 to enable a barrel cover 13 to move up and down integrally, stirring the whole raw material uniformly, and discharging generated ethephon aqua through the discharge outlet 17 at the bottom end of the barrel body 15 after stirring; when the ethephon water aqua is continuously produced, the inner wall of the barrel body 15 needs to be cleaned, the second piston push rod 25 is controlled to move towards the outer side of the stirring blade 2 through the second hydraulic cylinder 16, the second piston push rod 25 applies pressure to the sealing plate 23, the sealing plate 23 moves towards the inside of the sealing groove 21 due to the fact that the side wall of the sealing plate 23 is an inclined wall, the baffle plate 22 applies pressure to the spring 20, the spring 20 is compressed, the second piston push rod 25 extends out of the outer side of the stirring blade 2, the cleaning brush 24 at one end of the second piston push rod 25 is in contact with the inner wall of the barrel body 15, the first piston push rod 5 in the first hydraulic cylinder 4 controller moves up and down, the barrel cover 13 moves up and down integrally, meanwhile, clear water is added from the dosing port 7 and the feeding port 12, and the cleaning brush 24 fully cleans; after the cleaning is finished, the second piston push rod 25 is controlled by the second hydraulic cylinder 16 to move towards the inner side of the stirring blade 2, so that the cleaning brush 24 retracts into the rectangular groove 26, the spring 20 applies elasticity to the baffle 22, the sealing plate 23 moves downwards to block the notch of the rectangular groove 26, the raw materials are prevented from entering, the diester phosphate and other raw materials are added again, and the continuous production of the ethephon aqua is realized.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (1)
1. A preparation process for continuously producing a ethephon aqua is characterized by comprising the following steps:
the method comprises the following steps: adding 500g of phosphorus trichloride into a reaction kettle in an environment of-5 ℃, introducing ethylene oxide into the reaction kettle, keeping the temperature at 30 ℃, stirring for 3 hours, sampling for assay, taking materials when free chlorine reaches 0.1-0.3mg/kg, or else continuing introducing ethylene oxide, stirring for 30 minutes, sampling for assay, taking materials when the free chlorine reaches 0.1-0.3mg/kg, or else repeating the operation until the free chlorine reaches 0.1-0.3 mg/kg;
step two: heating the product in the step one to enable the temperature of the product to reach 240-250 ℃, and stirring for 20 minutes to obtain the diester phosphate;
step three: the phosphoric acid diester is injected into the barrel body (15) from the interior of a feed inlet (12) in the stirring device, heating the barrel body (15) to 175 ℃, introducing hydrogen chloride gas into the discharge hole (17) to fully react until dichloroethane is not generated, stopping introducing the hydrogen chloride gas, injecting water into the barrel body (15) through the medicine adding hole (7), driving the stirring shaft (14) to rotate by the output end of the motor (9) through the coupler, driving the stirring blades (2) at the bottom of the stirring shaft (14) to rotate when the stirring shaft (14) rotates, the raw materials in the barrel body (15) are stirred and move up and down through a first piston push rod (5) in a controller of a first hydraulic cylinder (4), the barrel cover (13) is integrally moved up and down, so that the raw materials are integrally stirred, the stirring is more uniform, and after the stirring is finished, the generated ethephon aqua is discharged through a discharge hole (17) at the bottom end of the barrel body (15);
step four: when the ethephon water aqua is continuously produced, the inner wall of a barrel body (15) needs to be cleaned, a second piston push rod (25) is controlled to move towards the outer side of a stirring blade (2) through a second hydraulic cylinder (16), the second piston push rod (25) applies pressure to a sealing plate (23), the sealing plate (23) moves towards the inner part of a sealing groove (21) due to the fact that the side wall of the sealing plate (23) is an inclined wall, a baffle plate (22) applies pressure to a spring (20) to compress the spring (20), the second piston push rod (25) extends out of the outer side of the stirring blade (2), a cleaning brush (24) at one end of the second piston push rod (25) is in contact with the inner wall of the barrel body (15), the barrel cover (13) integrally moves up and down through a first piston push rod (5) in a controller of a first hydraulic cylinder (4), and clear water is added from a medicine adding port (7) and a material adding port (12), the cleaning brush (24) fully cleans the whole inner wall of the barrel body (15);
step five: after cleaning, the second piston push rod (25) is controlled to move towards the inner side of the stirring blade (2) through the second hydraulic cylinder (16), so that the cleaning brush (24) retracts into the rectangular groove (26), the spring (20) exerts elastic force on the baffle (22), the sealing plate (23) moves downwards, the notch of the rectangular groove (26) is blocked, raw materials are prevented from entering, diester phosphate and other raw materials are added again, and continuous production of the ethephon aqua is achieved.
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| CN112717460A (en) * | 2020-12-16 | 2021-04-30 | 鼎泰（湖北）生化科技设备制造有限公司 | Easily abluent extraction tank |
| CN115610934A (en) * | 2022-12-12 | 2023-01-17 | 烟台通润化工科技有限公司 | Transport container for chemicals |
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| CN103250696A (en) * | 2013-04-12 | 2013-08-21 | 绍兴市东湖生化有限公司 | Preparation method for high-concentration ethephon aqua |
| CN207769775U (en) * | 2017-12-04 | 2018-08-28 | 潍坊天方圣鸿化学有限公司 | Neutralization reaction kettle with internal cleaning function |
| CN108970564A (en) * | 2017-06-05 | 2018-12-11 | 广西明福科技有限公司 | A kind of large capacity reaction kettle easy to clean |
| CN109529683A (en) * | 2018-11-29 | 2019-03-29 | 河南易成新能源股份有限公司 | The mixing arrangement and stirring means stirred evenly |
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| US9877480B2 (en) * | 2015-05-19 | 2018-01-30 | Valent Biosciences Llc | (S)-abscisic acid derivatives for enhanced grape coloration |
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|---|---|---|---|---|
| CN1048043A (en) * | 1989-06-14 | 1990-12-26 | 上海市农药研究所 | The preparation method of 2 chloroethyl phosphoric acid |
| CN103250696A (en) * | 2013-04-12 | 2013-08-21 | 绍兴市东湖生化有限公司 | Preparation method for high-concentration ethephon aqua |
| CN108970564A (en) * | 2017-06-05 | 2018-12-11 | 广西明福科技有限公司 | A kind of large capacity reaction kettle easy to clean |
| CN207769775U (en) * | 2017-12-04 | 2018-08-28 | 潍坊天方圣鸿化学有限公司 | Neutralization reaction kettle with internal cleaning function |
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Address after: 242200 Xinhang caijiashan Guangxin Industrial Park, Guangde County, Xuancheng City, Anhui Province Patentee after: Anhui Jiesheng Biotechnology Co.,Ltd. Address before: 242200 Xinhang caijiashan Guangxin Industrial Park, Guangde County, Xuancheng City, Anhui Province Patentee before: SUNONG (GUANGDE) BIOTECHNOLOGY Co.,Ltd. |