CN110150268A - A kind of ethephon agent and its preparation process - Google Patents
A kind of ethephon agent and its preparation process Download PDFInfo
- Publication number
- CN110150268A CN110150268A CN201910434896.7A CN201910434896A CN110150268A CN 110150268 A CN110150268 A CN 110150268A CN 201910434896 A CN201910434896 A CN 201910434896A CN 110150268 A CN110150268 A CN 110150268A
- Authority
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- China
- Prior art keywords
- staving
- parts
- push rod
- piston push
- cleaning
- 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.)
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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 44
- 239000005976 Ethephon Substances 0.000 title claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims description 26
- 238000004140 cleaning Methods 0.000 claims abstract description 64
- 238000003756 stirring Methods 0.000 claims abstract description 45
- 239000002994 raw material Substances 0.000 claims abstract description 41
- 238000007789 sealing Methods 0.000 claims abstract description 38
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 34
- 239000010452 phosphate Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000007789 gas Substances 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 11
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002347 injection Methods 0.000 claims abstract description 5
- 239000007924 injection Substances 0.000 claims abstract description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 23
- 239000000460 chlorine Substances 0.000 claims description 23
- 229910052801 chlorine Inorganic materials 0.000 claims description 23
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000005070 sampling Methods 0.000 claims description 13
- 230000008878 coupling Effects 0.000 claims description 12
- 238000010168 coupling process Methods 0.000 claims description 12
- 238000005859 coupling reaction Methods 0.000 claims description 12
- 230000006835 compression Effects 0.000 claims description 7
- 238000007906 compression Methods 0.000 claims description 7
- 238000010924 continuous production Methods 0.000 claims description 7
- 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 class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 5
- 238000009423 ventilation Methods 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 7
- 239000000243 solution Substances 0.000 description 5
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 3
- 239000007983 Tris buffer Substances 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ANHAEBWRQNIPEV-UHFFFAOYSA-N 2-chloroethyl dihydrogen phosphate Chemical compound OP(O)(=O)OCCCl ANHAEBWRQNIPEV-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- -1 chloroethenes Alkane Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process 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
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
Abstract
The invention discloses a kind of ethephon agent, ethephon agent is made of the parts by weight of the following raw material: the parts by weight of di-phosphate ester are 80-100 parts, and the parts by weight of hydrogen chloride gas are 10-30 parts, and the parts by weight of water are 30-50 parts；By di-phosphate ester inside the feed opening in agitating device inside injection staving, staving is heated, cleaning brush integrally carries out abundant cleaning to the inner wall of staving, after the completion of cleaning, medial movement of the second piston push rod to paddle is controlled by second hydraulic cylinder, so that the inside of cleaning brush retraction rectangular channel, spring applies elastic force to baffle, so that sealing plate moves down, block the notch of rectangular channel, raw material is avoided to enter, inner wall of barrel cleaning can be carried out after the completion of each stirring, guarantee material allocation precision, worker's Manual-cleaning is not needed, save physical strength, and guarantee that inner wall of barrel can be cleaned integrally, improve cleaning effect.
Description
Technical field
The present invention relates to the preparation field of ethephon (CEPHA),2-(chloroethyl) phosphonic acid, specially a kind of ethephon agent and its preparation process.
Background technique
The entitled 2 chloroethyl phosphoric acid of chemistry of ethephon (CEPHA),2-(chloroethyl) phosphonic acid, it is water-soluble preferable, it is used on crops, generallys use water
40% ethephon agent is widely used in agent at present.In order to reduce the cost of packaging and transport, using effect, factory are improved
Family tries to improve the concentration of ethephon agent.
It needs in ethephon agent preparation at present using di-phosphate ester, but in the preparation process of di-phosphate ester, needs
Enough ethylene oxide is usually disposably incorporated to phosphorus trichloride, then detects the mass fraction of free chlorine, leads to phosphorus trichloride
Waste, and in the preparation of ethephon agent, when needing to continue processing, it is necessary to which the last time container of processing is cleaned, and mesh
Preceding cleaning container needs artificial cleaning, or is cleaned using hydraulic giant, and cleaning is caused to be not thorough, and influences to deploy precision, cleaning is difficult.
Summary of the invention
The purpose of the present invention is to provide a kind of ethephon agent and its preparation processes, to solve current ethephon agent system
It needs in standby using di-phosphate ester, but in the preparation process of di-phosphate ester, needs usually disposably to incorporate phosphorus trichloride
Enough ethylene oxide, then the mass fraction of free chlorine is detected, lead to the waste of phosphorus trichloride, and in the preparation of ethephon agent
In, when needing to continue processing, it is necessary to the last time container of processing is cleaned, and cleaning container needs artificial cleaning at present, or
Person is cleaned using hydraulic giant, and cleaning is caused to be not thorough, and is influenced to deploy precision, is cleaned difficult problem.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of ethephon agent, the ethephon agent are made of the parts by weight of the following raw material:
The parts by weight of di-phosphate ester are 80-100 parts, and the parts by weight of hydrogen chloride gas are 10-30 parts, the parts by weight of water
Number is 30-50 parts；
The di-phosphate ester is made by the steps:
Step 1: by the environment of -5 DEG C, 500g phosphorus trichloride is added in reaction kettle, epoxy is passed through into reaction kettle
Ethane, is stirred work by 30 DEG C of constant temperature, and after stirring 3 hours, sampling is chemically examined, and reaches 0.1-0.3mg/kg in free chlorine
When, can feeding, no person is further continued for being passed through ethylene oxide, while after stirring 30 minutes, sampling is chemically examined, and is reached in free chlorine
When 0.1-0.3mg/kg, can feeding, otherwise, repeat it is above-mentioned complies, until free chlorine reaches 0.1-0.3mg/kg；
Step 2: addition processing is carried out to the product in step 1, its temperature is made to reach 240-250 DEG C, is stirred place
Reason, mixing time are 20 minutes, obtain di-phosphate ester；
The ethephon agent is prepared by the following procedure technique and is prepared:
Di-phosphate ester inside injection staving, heats staving, reach it inside the feed opening in agitating device
To 175 DEG C, discharge port is passed through hydrogen chloride gas, reacts it sufficiently, and until dichloroethanes is not generating, stopping is ventilated, then is led to
It crosses dosing mouth and injects water to the inside of staving, the output end of motor drives agitating shaft to rotate by shaft coupling, and agitating shaft turns
When dynamic, drive the paddle of its bottom to rotate, work is stirred to the raw material inside staving, passes through first hydraulic cylinder controller
Its internal first piston push rod moves up and down, so that bung integrally moves up and down, so that raw material is integrally stirred,
So that stirring is more uniform, after the completion of stirring, the ethephon agent of generation is discharged by the discharge port of staving bottom end, is completed to second
The preparation work of alkene benefit aqua.
As a further solution of the present invention: in the preparation process of the di-phosphate ester, epoxy second is passed through into reaction kettle
Alkane, is stirred work by 30 DEG C of constant temperature, and after stirring 3 hours, sampling is chemically examined, when free chlorine reaches 0.1-0.3mg/kg,
Can feeding, no person is further continued for being passed through ethylene oxide, while after stirring 30 minutes, sampling is chemically examined, and is reached in free chlorine
When 0.1-0.3mg/kg, can feeding, otherwise, repeat it is above-mentioned complies, it is straight with tradition until free chlorine reaches 0.1-0.3mg/kg
It connects and is compared into enough ethylene oxide, the dosage of ethylene oxide can be saved.
As a further solution of the present invention: in the logical preparation process of the di-phosphate ester, reaction temperature 240-250
DEG C, then be stirred, mixing time is 20 minutes, so that tris phosphite generates di-phosphate ester, guarantees that reaction is more thorough
Bottom.
A kind of preparation process of ethephon agent, the preparation process specifically includes the following steps:
S1: di-phosphate ester inside injection staving, heats staving, makes it inside the feed opening in agitating device
Reach 175 DEG C, discharge port is passed through hydrogen chloride gas, reacts it sufficiently, and until dichloroethanes is not generating, stopping is ventilated；
S2: water is injected to the inside of staving by dosing mouth again, the output end of motor drives agitating shaft hair by shaft coupling
Raw rotation drives the paddle of its bottom to rotate, is stirred work to the raw material inside staving, passes through when agitating shaft rotates
Its internal first piston push rod of first hydraulic cylinder controller moves up and down, so that bung integrally moves up and down, so that former
Material is whole to be stirred, so that stirring is more uniform, after the completion of stirring, ethephon agent the going out by staving bottom end of generation
Material mouth discharge；
S3: it in continuous production ethephon agent, needs to clean the inner wall of staving, be controlled by second hydraulic cylinder
Second piston push rod is mobile to the outside of paddle, and second piston push rod applies pressure to sealing plate, due to the side wall of sealing plate
For inclined wall, so that sealing plate is mobile to the inside of seal groove, baffle applies pressure to spring, so that spring generates compression, the
Two piston push rods stretch out on the outside of paddle, and the cleaning brush of second piston push rod one end is contacted with the inner wall of staving, pass through the first liquid
Its internal first piston push rod of cylinder pressure controller moves up and down, so that bung integrally moves up and down, while from dosing mouth
Clear water is added with feed opening, cleaning brush integrally carries out abundant cleaning to the inner wall of staving；
S4: after the completion of cleaning, medial movement of the second piston push rod to paddle is controlled by second hydraulic cylinder, so that clearly
The inside of clean brush retraction rectangular channel, spring apply elastic force to baffle and block the notch of rectangular channel so that sealing plate moves down,
It avoids raw material from entering, di-phosphate ester and other raw materials is added again, realize the continuous production of ethephon agent.
As a further solution of the present invention: the agitating device includes pedestal, staving and sealing plate, the top of the pedestal
Portion is fixed with staving, and the bottom of staving is equipped with discharge port, and the outer surface of staving is equipped with securing plate, the top of the pedestal of staving surrounding
Four first hydraulic cylinders are respectively equipped on face, the inside of four first hydraulic cylinders is equipped with first piston push rod, the side wall top of staving
Position has installed lower cover, and the top of staving is equipped with bung, and the sidewall bottom of bung position corresponding with lower cover is equipped with upper end
Lid, is equipped with sealing joint strip between upper end cover and lower cover, the medium position of bung top surface is welded with mounting rack, the side of mounting rack
Equipped with feed opening, the other side of mounting rack is equipped with dosing mouth, and the top of feed opening is equipped with capping, and capping is equipped with handle, bung
It is welded with and is set there are four horizontal axis on side wall, the top of four first piston push rods is fixedly connected with the bottom surface of horizontal axis, mounting rack
Top is fixedly installed with motor, and the bottom of motor is equipped with agitating shaft, and the output end of motor passes through the top of shaft coupling and agitating shaft
Transmission connection, the bottom end of agitating shaft pass through the inside that bung protrudes into staving, and the bottom end of agitating shaft is equipped with paddle, and the two of paddle
Rectangular channel is offered inside end structure, the inside of two rectangular channels is respectively equipped with second hydraulic cylinder, and the inside of second hydraulic cylinder is set
There is second piston push rod, one end of second piston push rod is set on the inner wall of second hydraulic cylinder and the end face of second piston push rod
There is cleaning brush, the inside of the paddle above cleaning brush offers seal groove, and the inside of seal groove is equipped with baffle, the side of baffle
It is fixedly connected with sealing plate, the side wall of sealing plate side adjacent with cleaning brush is inclined wall, the other side of baffle and seal groove
Be equipped with spring between inner wall, in use, opening capping by handle, raw material injected inside the feed opening, then pass through dosing mouth to
Another raw material is injected in the inside of staving, and the output end of motor drives agitating shaft to rotate by shaft coupling, agitating shaft rotation
When, drive the paddle of its bottom to rotate, work be stirred to the raw material inside staving, by first hydraulic cylinder controller its
Internal first piston push rod moves up and down, so that bung integrally moves up and down, so that raw material is integrally stirred, makes
It must stir more uniform, after the completion of stirring, be discharged by the discharge port of staving bottom end, when needing to be again stirring for raw material, be needed pair
The inner wall of staving is cleaned, and controls second piston push rod to the movement of the outside of paddle, second piston by second hydraulic cylinder
Push rod applies pressure to sealing plate, since the side wall of sealing plate is inclined wall, so that sealing plate is mobile to the inside of seal groove, gear
Plate applies pressure to spring, so that spring generates compression, second piston push rod stretches out on the outside of paddle, second piston push rod one end
Cleaning brush contacted with the inner wall of staving, by first hydraulic cylinder controller, its internal first piston push rod is moved up and down, and is made
Bung integrally moves up and down, while being added clear water from dosing mouth and feed opening, cleaning brush it is whole to the inner wall of staving into
Row abundant cleaning after the completion of cleaning, controls medial movement of the second piston push rod to paddle by second hydraulic cylinder, makes
The inside of cleaning brush retraction rectangular channel is obtained, spring applies elastic force to baffle and blocks the slot of rectangular channel so that sealing plate moves down
Mouthful, it avoids raw material from entering, inner wall of barrel cleaning can be carried out after the completion of each stirring, guarantee material allocation precision, no
Worker's Manual-cleaning is needed, physical strength is saved, and guarantees that inner wall of barrel can be cleaned integrally, improves cleaning effect.
Beneficial effects of the present invention:
1, in the present invention, in the preparation process of di-phosphate ester, it is passed through ethylene oxide into reaction kettle, 30 DEG C of constant temperature, carries out
Stir work, stirring 3 hours after, sampling chemically examined, when free chlorine reaches 0.1-0.3mg/kg, can feeding, no person is again
Continue to be passed through ethylene oxide, while after stirring 30 minutes, sampling is chemically examined, when free chlorine reaches 0.1-0.3mg/kg, i.e.,
Can feeding, otherwise, repeat it is above-mentioned complies, until free chlorine reaches 0.1-0.3mg/kg, be passed directly into enough epoxies with tradition
Ethane is compared, and the dosage of ethylene oxide can be saved；
2, in the present invention, the output end of motor drives agitating shaft to rotate by shaft coupling, when agitating shaft rotates, driving
The paddle of its bottom rotates, and is stirred work to the raw material inside staving, passes through its inside of first hydraulic cylinder controller
First piston push rod moves up and down, so that bung integrally moves up and down, so that raw material is integrally stirred, so that stirring
It is more uniform, after the completion of stirring, it is discharged by the discharge port of staving bottom end, when needing to be again stirring for raw material, is needed to staving
Inner wall is cleaned, and controls second piston push rod to the movement of the outside of paddle, second piston push rod pair by second hydraulic cylinder
Sealing plate applies pressure, and since the side wall of sealing plate is inclined wall, so that sealing plate is mobile to the inside of seal groove, baffle is to bullet
Spring applies pressure, so that spring generates compression, second piston push rod stretches out on the outside of paddle, the cleaning of second piston push rod one end
Brush is contacted with the inner wall of staving, and by first hydraulic cylinder controller, its internal first piston push rod is moved up and down, so that bung
Entirety moves up and down, while clear water is added from dosing mouth and feed opening, and cleaning brush integrally carries out sufficiently the inner wall of staving
Cleaning after the completion of cleaning, controls medial movement of the second piston push rod to paddle by second hydraulic cylinder, so that cleaning
The inside of brush retraction rectangular channel, spring apply elastic force to baffle and block the notch of rectangular channel so that sealing plate moves down, keep away
Exempt from raw material entrance, inner wall of barrel cleaning can be carried out after the completion of each stirring, guarantee material allocation precision, do not need work
People's Manual-cleaning saves physical strength, and guarantees that inner wall of barrel can be cleaned integrally, improves cleaning effect.
Detailed description of the invention
In order to facilitate the understanding of those skilled in the art, the present invention will be further described below with reference to the drawings.
Fig. 1 is the structural schematic diagram of agitating device in the present invention；
Fig. 2 is the top view of agitating device in the present invention；
Fig. 3 is the partial enlarged view A in the present invention；
Fig. 4 is the partial enlarged view B in the present invention；
In figure: 1, pedestal；2, paddle；3, securing plate；4, first hydraulic cylinder；5, first piston push rod；6, horizontal axis；7, add
Medicine mouth；8, mounting rack；9, motor；10, it covers；11, handle；12, feed opening；13, bung；14, agitating shaft；15, staving；16,
Second hydraulic cylinder；17, discharge port；18, upper end cover；19, lower cover；20, spring；21, seal groove；22, baffle；23, sealing plate；
24, cleaning brush；25, second piston push rod；26, rectangular channel.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with embodiment, it is clear that described reality
Applying example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff all other embodiment obtained without creative efforts belongs to what the present invention protected
Range.
As shown in Figs 1-4, a kind of ethephon agent, the ethephon agent are made of the parts by weight of the following raw material:
The parts by weight of di-phosphate ester are 80-100 parts, and the parts by weight of hydrogen chloride gas are 10-30 parts, the parts by weight of water
Number is 30-50 parts；
The di-phosphate ester is made by the steps:
Step 1: by the environment of -5 DEG C, 500g phosphorus trichloride is added in reaction kettle, epoxy is passed through into reaction kettle
Ethane, is stirred work by 30 DEG C of constant temperature, and after stirring 3 hours, sampling is chemically examined, and reaches 0.1-0.3mg/kg in free chlorine
When, can feeding, no person is further continued for being passed through ethylene oxide, while after stirring 30 minutes, sampling is chemically examined, and is reached in free chlorine
When 0.1-0.3mg/kg, can feeding, otherwise, repeat it is above-mentioned complies, until free chlorine reaches 0.1-0.3mg/kg；
Step 2: addition processing is carried out to the product in step 1, its temperature is made to reach 240-250 DEG C, is stirred place
Reason, mixing time are 20 minutes, obtain di-phosphate ester；
The ethephon agent is prepared by the following procedure technique and is prepared:
Di-phosphate ester is injected inside staving 15 inside the feed opening 12 in agitating device, staving 15 is heated,
175 DEG C are reached, discharge port 17 is passed through hydrogen chloride gas, reacts it sufficiently, and until dichloroethanes is not generating, stopping is logical
Gas, then water is injected to the inside of staving 15 by dosing mouth 7, the output end of motor 9 drives agitating shaft 14 to occur by shaft coupling
Rotation drives the paddle 2 of its bottom to rotate, is stirred work to the raw material inside staving 15 when agitating shaft 14 rotates, and leads to
The first piston push rod 5 for crossing its inside of 4 controller of first hydraulic cylinder moves up and down, and moves up and down so that bung 13 is whole,
So that raw material is integrally stirred, so that stirring is more uniform, after the completion of stirring, the ethephon agent of generation passes through staving 15
The discharge port 17 of bottom end is discharged, and completes the preparation work to ethephon agent.
In the preparation process of di-phosphate ester, it is passed through ethylene oxide into reaction kettle, 30 DEG C of constant temperature, is stirred work, stirs
After mixing 3 hours, sampling is chemically examined, when free chlorine reaches 0.1-0.3mg/kg, can feeding, no person is further continued for being passed through epoxy
Ethane, at the same stir 30 minutes after, sampling chemically examined, when free chlorine reaches 0.1-0.3mg/kg, can feeding, otherwise,
Repetition is above-mentioned to be complied, until free chlorine reaches 0.1-0.3mg/kg, it, can compared with tradition is passed directly into enough ethylene oxide
Save the dosage of ethylene oxide.
In the logical preparation process of di-phosphate ester, reaction temperature is 240-250 DEG C, then is stirred, and mixing time is
20 minutes, so that tris phosphite generates di-phosphate ester, guarantee that reaction is more thorough.
A kind of preparation process of ethephon agent, the preparation process specifically includes the following steps:
S1: di-phosphate ester is injected inside staving 15 inside the feed opening 12 in agitating device, staving 15 is added
Heat reaches 175 DEG C, and discharge port 17 is passed through hydrogen chloride gas, reacts it sufficiently, until dichloroethanes is not generating, stops
Only ventilate；
S2: water is injected to the inside of staving 15 by dosing mouth 7 again, the output end of motor 9 is driven by shaft coupling to be stirred
Axis 14 rotates, and when agitating shaft 14 rotates, drives the paddle 2 of its bottom to rotate, stirs the raw material inside staving 15
Work is mixed, its internal first piston push rod 5 moves up and down by 4 controller of first hydraulic cylinder, carries out so that bung 13 is whole
It moves up and down, so that raw material is integrally stirred, so that stirring is more uniform, after the completion of stirring, the ethephon agent of generation
It is discharged by the discharge port 17 of 15 bottom end of staving；
S3: it in continuous production ethephon agent, needs the inner wall to staving 15 to clean, passes through second hydraulic cylinder 16
It is mobile to the outside of paddle 2 to control second piston push rod 25, second piston push rod 25 applies pressure to sealing plate 23, due to close
The side wall of sealing plate 23 is inclined wall, so that sealing plate 23 is mobile to the inside of seal groove 21, baffle 22 applies pressure to spring 20,
So that spring 20 generates compression, second piston push rod 25 stretches out 2 outside of paddle, the cleaning brush 24 of 25 one end of second piston push rod
It is contacted with the inner wall of staving 15, by 4 controller of first hydraulic cylinder, its internal first piston push rod 5 is moved up and down, so that bucket
Lid 13 is whole to be moved up and down, while clear water is added from dosing mouth 7 and feed opening 12, and cleaning brush 24 is whole to the inner wall of staving 15
Body carries out abundant cleaning；
S4: after the completion of cleaning, controlling medial movement of the second piston push rod 25 to paddle 2 by second hydraulic cylinder 16,
So that the inside of 24 retraction rectangular channel 26 of cleaning brush, spring 20 applies elastic force to baffle 22, so that sealing plate 23 moves down, blocks up
The firmly notch of rectangular channel 26, avoids raw material from entering, and di-phosphate ester and other raw materials are added again, realize continuing for ethephon agent
Production.
Agitating device includes pedestal 1, staving 15 and sealing plate 23, and the top of the pedestal 1 is fixed with staving 15, staving
15 bottom is equipped with discharge port 17, and the outer surface of staving 15 is equipped with securing plate 3, distinguishes on the top surface of the pedestal 1 of 15 surrounding of staving
If the inside of four first hydraulic cylinders 4 is equipped with first piston push rod 5, the top side wall position of staving 15 there are four first hydraulic cylinder 4
Lower cover 19 is installed, the top of staving 15 is equipped with bung 13, and the sidewall bottom of bung 13 position corresponding with lower cover 19 is set
There is upper end cover 18, sealing joint strip is equipped between upper end cover 18 and lower cover 19, the medium position of 13 top surface of bung is welded with installation
Frame 8, the side of mounting rack 8 are equipped with feed opening 12, and the other side of mounting rack 8 is equipped with dosing mouth 7, and the top of feed opening 12 is equipped with envelope
Lid 10, capping 10 are equipped with handle 11, horizontal axis 6 there are four setting, the top of four first piston push rods 5 are welded on 13 side wall of bung
End is fixedly connected with the bottom surface of horizontal axis 6, and the top of mounting rack 8 is fixedly installed with motor 9, and the bottom of motor 9 is equipped with agitating shaft 14,
The output end of motor 9 is sequentially connected by the top of shaft coupling and agitating shaft 14, and the bottom end of agitating shaft 14 passes through bung 13 and protrudes into
The inside of staving 15, the bottom end of agitating shaft 14 are equipped with paddle 2, offer rectangular channel 26 inside the two-end structure of paddle 2, and two
The inside of a rectangular channel 26 is respectively equipped with second hydraulic cylinder 16, and the inside of second hydraulic cylinder 16 is equipped with second piston push rod 25, the
One end of two piston push rods 25 passes through the inner wall of second hydraulic cylinder 16 and the end face of second piston push rod 25 is equipped with cleaning brush 24,
The inside of the paddle 2 of the top of cleaning brush 24 offers seal groove 21, and the inside of seal groove 21 is equipped with baffle 22, and the one of baffle 22
Side is fixedly connected with sealing plate 23, and the side wall of the side adjacent with cleaning brush 24 of sealing plate 23 is inclined wall, the other side of baffle 22
It is equipped with spring 20 between the inner wall of seal groove 21, in use, opening capping 10 by handle 11, is injected inside feed opening 12
Raw material, then another raw material is injected to the inside of staving 15 by dosing mouth 7, the output end of motor 9 is stirred by shaft coupling driving
It mixes axis 14 to rotate, when agitating shaft 14 rotates, the paddle 2 of its bottom is driven to rotate, the raw material inside staving 15 is carried out
Stir work, by 4 controller of first hydraulic cylinder, its internal first piston push rod 5 is moved up and down so that bung 13 it is whole into
Row moves up and down, so that raw material is integrally stirred, so that stirring is more uniform, after the completion of stirring, passes through 15 bottom end of staving
Discharge port 17 be discharged, when needing to be again stirring for raw material, need the inner wall to staving 15 to clean, pass through second hydraulic cylinder 16
It is mobile to the outside of paddle 2 to control second piston push rod 25, second piston push rod 25 applies pressure to sealing plate 23, due to close
The side wall of sealing plate 23 is inclined wall, so that sealing plate 23 is mobile to the inside of seal groove 21, baffle 22 applies pressure to spring 20,
So that spring 20 generates compression, second piston push rod 25 stretches out 2 outside of paddle, the cleaning brush 24 of 25 one end of second piston push rod
It is contacted with the inner wall of staving 15, by 4 controller of first hydraulic cylinder, its internal first piston push rod 5 is moved up and down, so that bucket
Lid 13 is whole to be moved up and down, while clear water is added from dosing mouth 7 and feed opening 12, and cleaning brush 24 is whole to the inner wall of staving 15
Body carries out abundant cleaning, after the completion of cleaning, controls second piston push rod 25 into paddle 2 by second hydraulic cylinder 16
Side is mobile, so that the inside of 24 retraction rectangular channel 26 of cleaning brush, spring 20 applies elastic force to baffle 22, so that sealing plate 23 is downward
It is mobile, the notch of rectangular channel 26 is blocked, raw material is avoided to enter, 15 inner wall washing work of staving can be carried out after the completion of each stirring
Make, guarantee material allocation precision, do not need worker's Manual-cleaning, save physical strength, and guarantees that 15 inner wall of staving can be carried out integrally
Cleaning improves cleaning effect.
The working principle of the invention: di-phosphate ester is injected inside staving 15 inside the feed opening 12 in agitating device,
Staving 15 is heated, reaches 175 DEG C, discharge port 17 is passed through hydrogen chloride gas, reacts it sufficiently, until two chloroethenes
Alkane is not generating, and stops ventilation；Water is injected to the inside of staving 15 by dosing mouth 7 again, the output end of motor 9 passes through shaft coupling
Driving agitating shaft 14 rotates, and when agitating shaft 14 rotates, drives the paddle 2 of its bottom to rotate, to the original inside staving 15
Material is stirred work, and by 4 controller of first hydraulic cylinder, its internal first piston push rod 5 is moved up and down, so that bung 13
Entirety moves up and down, so that raw material is integrally stirred, so that stirring is more uniform, after the completion of stirring, the second of generation
Alkene benefit aqua is discharged by the discharge port 17 of 15 bottom end of staving；In continuous production ethephon agent, need in staving 15
Wall is cleaned, and controls second piston push rod 25 to the movement of the outside of paddle 2, second piston push rod by second hydraulic cylinder 16
25 pairs of sealing plates 23 apply pressure, since the side wall of sealing plate 23 is inclined wall, so that sealing plate 23 is to the inside of seal groove 21
Mobile, baffle 22 applies pressure to spring 20, so that spring 20 generates compression, second piston push rod 25 stretches out 2 outside of paddle,
The cleaning brush 24 of 25 one end of second piston push rod is contacted with the inner wall of staving 15, passes through its inside of 4 controller of first hydraulic cylinder
First piston push rod 5 moves up and down, and moves up and down so that bung 13 is whole, while being added from dosing mouth 7 and feed opening 12
Clear water, cleaning brush 24 integrally carry out abundant cleaning to the inner wall of staving 15；After the completion of cleaning, controlled by second hydraulic cylinder 16
Second piston push rod 25 processed is to the medial movement of paddle 2, so that the inside of 24 retraction rectangular channel 26 of cleaning brush, 20 pairs of spring are kept off
Plate 22 applies elastic force and blocks the notch of rectangular channel 26 so that sealing plate 23 moves down, raw material is avoided to enter, phosphorus is added again
Acid diesters and other raw materials, realize the continuous production of ethephon agent.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (4)
1. a kind of ethephon agent, which is characterized in that the ethephon agent is made of the parts by weight of the following raw material:
The parts by weight of di-phosphate ester are 80-100 parts, and the parts by weight of hydrogen chloride gas are 10-30 parts, and the parts by weight of water are
30-50 parts；
The di-phosphate ester is made by the steps:
Step 1: by the environment of -5 DEG C, 500g phosphorus trichloride is added in reaction kettle, epoxy second is passed through into reaction kettle
Alkane, is stirred work by 30 DEG C of constant temperature, and after stirring 3 hours, sampling is chemically examined, when free chlorine reaches 0.1-0.3mg/kg,
Can feeding, no person is further continued for being passed through ethylene oxide, while after stirring 30 minutes, sampling is chemically examined, and is reached in free chlorine
When 0.1-0.3mg/kg, can feeding, otherwise, repeat it is above-mentioned complies, until free chlorine reaches 0.1-0.3mg/kg；
Step 2: addition processing is carried out to the product in step 1, so that its temperature is reached 240-250 DEG C, is stirred, stir
Mixing the time is 20 minutes, obtains di-phosphate ester；
The ethephon agent is prepared by the following procedure technique and is prepared:
By di-phosphate ester, injection staving (15) is internal inside the feed opening (12) in agitating device, adds to staving (15)
Heat reaches 175 DEG C, and discharge port (17) is passed through hydrogen chloride gas, reacts it sufficiently, until dichloroethanes is not generating,
Stop ventilation, then inject water to the inside of staving (15) by dosing mouth (7), the output end of motor (9) is driven by shaft coupling
Agitating shaft (14) rotates, and when agitating shaft (14) rotates, the paddle (2) of its bottom is driven to rotate, internal to staving (15)
Raw material be stirred work, by first hydraulic cylinder (4) controller, its internal first piston push rod (5) is moved up and down, and is made
It obtains bung (13) integrally to move up and down, so that raw material is integrally stirred, so that stirring is more uniform, stirring is completed
Afterwards, the ethephon agent of generation is discharged by the discharge port (17) of staving (15) bottom end, completes the preparation work to ethephon agent
Make.
2. a kind of ethephon agent according to claim 1, which is characterized in that in the preparation process of the di-phosphate ester,
It is passed through ethylene oxide into reaction kettle, 30 DEG C of constant temperature, is stirred work, after stirring 3 hours, sampling is chemically examined, free
When chlorine reaches 0.1-0.3mg/kg, can feeding, no person is further continued for being passed through ethylene oxide, while after stirring 30 minutes, sample into
Row chemical examination, when free chlorine reaches 0.1-0.3mg/kg, can feeding, otherwise, repeat it is above-mentioned complies, until free chlorine reaches
0.1-0.3mg/kg。
3. a kind of ethephon agent according to claim 1, which is characterized in that the logical preparation process of the di-phosphate ester
In, reaction temperature is 240-250 DEG C, then is stirred, and mixing time is 20 minutes.
4. a kind of preparation process of ethephon agent, which is characterized in that the preparation process specifically includes the following steps:
S1: by di-phosphate ester, injection staving (15) is internal inside the feed opening (12) in agitating device, carries out to staving (15)
Heating, reaches 175 DEG C, discharge port (17) is passed through hydrogen chloride gas, reacts it sufficiently, until dichloroethanes is not in life
At stopping ventilation；
S2: water is injected to the inside of staving (15) by dosing mouth (7) again, the output end of motor (9) is stirred by shaft coupling driving
It mixes axis (14) to rotate, when agitating shaft (14) rotates, the paddle (2) of its bottom is driven to rotate, internal to staving (15)
Raw material is stirred work, and by first hydraulic cylinder (4) controller, its internal first piston push rod (5) is moved up and down, so that
Bung (13) integrally moves up and down, so that raw material is integrally stirred, so that stirring is more uniform, and after the completion of stirring,
The ethephon agent of generation is discharged by the discharge port (17) of staving (15) bottom end；
S3: it in continuous production ethephon agent, needs the inner wall to staving (15) to clean, passes through second hydraulic cylinder (16)
Second piston push rod (25) are controlled to the movement of the outside of paddle (2), second piston push rod (25), which applies sealing plate (23), presses
Power, since the side wall of sealing plate (23) is inclined wall, so that sealing plate (23) is mobile to the inside of seal groove (21), baffle (22)
Pressure is applied to spring (20), so that spring (20) generates compression, second piston push rod (25) stretches out on the outside of paddle (2), the
The cleaning brush (24) of two piston push rods (25) one end is contacted with the inner wall of staving (15), by first hydraulic cylinder (4) controller its
Internal first piston push rod (5) moves up and down so that bung (13) integrally moves up and down, while from dosing mouth (7) and
Clear water is added in feed opening (12), and cleaning brush (24) integrally carries out abundant cleaning to the inner wall of staving (15)；
S4: after the completion of cleaning, the interior sidesway of second piston push rod (25) to paddle (2) is controlled by second hydraulic cylinder (16)
Dynamic, so that the inside of cleaning brush (24) retraction rectangular channel (26), spring (20) applies elastic force to baffle (22), so that sealing plate
(23) it moves down, blocks the notch of rectangular channel (26), raw material is avoided to enter, di-phosphate ester and other raw materials are added again, it is real
The continuous production of existing ethephon agent.
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| CN110150268B (en) | 2021-08-03 |
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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. |