CN115448828B - Production process of diphenyl ketone and safe working method in process - Google Patents
Production process of diphenyl ketone and safe working method in process Download PDFInfo
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- CN115448828B CN115448828B CN202211165295.9A CN202211165295A CN115448828B CN 115448828 B CN115448828 B CN 115448828B CN 202211165295 A CN202211165295 A CN 202211165295A CN 115448828 B CN115448828 B CN 115448828B
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- 238000000034 method Methods 0.000 title claims abstract description 69
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 139
- 230000007062 hydrolysis Effects 0.000 claims abstract description 73
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 73
- 238000005406 washing Methods 0.000 claims abstract description 64
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000000463 material Substances 0.000 claims abstract description 44
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 43
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 238000007599 discharging Methods 0.000 claims abstract description 33
- 239000003513 alkali Substances 0.000 claims abstract description 30
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000012965 benzophenone Substances 0.000 claims abstract description 19
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006552 photochemical reaction Methods 0.000 claims abstract description 7
- 239000002912 waste gas Substances 0.000 claims abstract description 6
- 238000011049 filling Methods 0.000 claims abstract description 5
- 238000002955 isolation Methods 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 238000004891 communication Methods 0.000 claims description 138
- 230000005540 biological transmission Effects 0.000 claims description 51
- 230000001105 regulatory effect Effects 0.000 claims description 28
- 230000001276 controlling effect Effects 0.000 claims description 22
- 238000004821 distillation Methods 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 18
- 238000003860 storage Methods 0.000 claims description 17
- VEFXTGTZJOWDOF-UHFFFAOYSA-N benzene;hydrate Chemical compound O.C1=CC=CC=C1 VEFXTGTZJOWDOF-UHFFFAOYSA-N 0.000 claims description 14
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 239000012074 organic phase Substances 0.000 claims description 10
- 235000010290 biphenyl Nutrition 0.000 claims description 9
- 239000004305 biphenyl Substances 0.000 claims description 9
- 230000003301 hydrolyzing effect Effects 0.000 claims description 8
- 239000012071 phase Substances 0.000 claims description 8
- 239000012267 brine Substances 0.000 claims description 7
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000012043 crude product Substances 0.000 claims description 6
- 239000013505 freshwater Substances 0.000 claims description 6
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000012795 verification Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 238000010992 reflux Methods 0.000 description 16
- 239000007789 gas Substances 0.000 description 13
- 238000009833 condensation Methods 0.000 description 10
- 230000005494 condensation Effects 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 8
- 238000005070 sampling Methods 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 4
- 238000012790 confirmation Methods 0.000 description 4
- 229910002056 binary alloy Inorganic materials 0.000 description 3
- 239000000686 essence Substances 0.000 description 3
- 230000003472 neutralizing effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 150000001447 alkali salts Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- ZCILODAAHLISPY-UHFFFAOYSA-N biphenyl ether Natural products C1=C(CC=C)C(O)=CC(OC=2C(=CC(CC=C)=CC=2)O)=C1 ZCILODAAHLISPY-UHFFFAOYSA-N 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 2
- 239000011552 falling film Substances 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- CIVCELMLGDGMKZ-UHFFFAOYSA-N 2,4-dichloro-6-methylpyridine-3-carboxylic acid Chemical compound CC1=CC(Cl)=C(C(O)=O)C(Cl)=N1 CIVCELMLGDGMKZ-UHFFFAOYSA-N 0.000 description 1
- WAASLNJSONWCGI-UHFFFAOYSA-N 4,4-dicyclohexylpiperidine Chemical compound C1(CCCCC1)C1(CCNCC1)C1CCCCC1 WAASLNJSONWCGI-UHFFFAOYSA-N 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- GIJXKZJWITVLHI-PMOLBWCYSA-N benzatropine Chemical compound O([C@H]1C[C@H]2CC[C@@H](C1)N2C)C(C=1C=CC=CC=1)C1=CC=CC=C1 GIJXKZJWITVLHI-PMOLBWCYSA-N 0.000 description 1
- 229960001081 benzatropine Drugs 0.000 description 1
- 235000014121 butter Nutrition 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 239000013058 crude material Substances 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229960000525 diphenhydramine hydrochloride Drugs 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 210000000582 semen Anatomy 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000008234 soft water Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/45—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation
- C07C45/47—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation using phosgene
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/45—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation
- C07C45/46—Friedel-Crafts reactions
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04L—TRANSMISSION OF DIGITAL INFORMATION, e.g. TELEGRAPHIC COMMUNICATION
- H04L63/00—Network architectures or network communication protocols for network security
- H04L63/04—Network architectures or network communication protocols for network security for providing a confidential data exchange among entities communicating through data packet networks
- H04L63/0428—Network architectures or network communication protocols for network security for providing a confidential data exchange among entities communicating through data packet networks wherein the data content is protected, e.g. by encrypting or encapsulating the payload
- H04L63/0442—Network architectures or network communication protocols for network security for providing a confidential data exchange among entities communicating through data packet networks wherein the data content is protected, e.g. by encrypting or encapsulating the payload wherein the sending and receiving network entities apply asymmetric encryption, i.e. different keys for encryption and decryption
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04L—TRANSMISSION OF DIGITAL INFORMATION, e.g. TELEGRAPHIC COMMUNICATION
- H04L67/00—Network arrangements or protocols for supporting network services or applications
- H04L67/01—Protocols
- H04L67/12—Protocols specially adapted for proprietary or special-purpose networking environments, e.g. medical networks, sensor networks, networks in vehicles or remote metering networks
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04W—WIRELESS COMMUNICATION NETWORKS
- H04W12/00—Security arrangements; Authentication; Protecting privacy or anonymity
- H04W12/03—Protecting confidentiality, e.g. by encryption
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04W—WIRELESS COMMUNICATION NETWORKS
- H04W12/00—Security arrangements; Authentication; Protecting privacy or anonymity
- H04W12/04—Key management, e.g. using generic bootstrapping architecture [GBA]
- H04W12/043—Key management, e.g. using generic bootstrapping architecture [GBA] using a trusted network node as an anchor
- H04W12/0431—Key distribution or pre-distribution; Key agreement
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04W—WIRELESS COMMUNICATION NETWORKS
- H04W12/00—Security arrangements; Authentication; Protecting privacy or anonymity
- H04W12/40—Security arrangements using identity modules
- H04W12/47—Security arrangements using identity modules using near field communication [NFC] or radio frequency identification [RFID] modules
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04L—TRANSMISSION OF DIGITAL INFORMATION, e.g. TELEGRAPHIC COMMUNICATION
- H04L2209/00—Additional information or applications relating to cryptographic mechanisms or cryptographic arrangements for secret or secure communication H04L9/00
- H04L2209/80—Wireless
- H04L2209/805—Lightweight hardware, e.g. radio-frequency identification [RFID] or sensor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Computer Security & Cryptography (AREA)
- Signal Processing (AREA)
- Computer Networks & Wireless Communication (AREA)
- Computing Systems (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
- Medical Informatics (AREA)
- Health & Medical Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Computer Hardware Design (AREA)
- General Engineering & Computer Science (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention provides a benzophenone production process and a safe working method in the process, comprising the following steps: s1, firstly, N is introduced 2 A to B times of replacement, wherein A, B is a positive integer of 2 or more and 5 or less, B>A, discharging the replacement waste gas to an alkali sealing tank; s2, slowly placing the prepared benzene in the benzene metering tank into an photochemical kettle; s3, slowly adding the prepared aluminum trichloride in the aluminum trichloride charging hopper into an photochemical kettle; s4, after the addition of benzene and aluminum trichloride is finished, starting an photochemical kettle for stirring; after stirring and running for a few minutes, if the temperature T of the photochemical kettle is less than or equal to the set temperature, opening jacket steam, and after the temperature of the photochemical kettle is increased to be more than or equal to the set temperature, closing a steam isolation valve on site of the photochemical kettle; s5, dropwise adding liquid phosgene into an photochemical kettle for photochemical reaction; s6, slowly filling N into the photochemical kettle 2 After the pressure is built, a discharging valve is slowly opened, and the material is discharged into the hydrolysis kettle;s7, a hydrolysis process; s8, a neutralization and water washing process; s9, a rectification step. The invention can play a protective role safely and avoid being attacked.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a benzophenone production process and a safe working method in the process.
Background
Benzophenone is an intermediate for ultraviolet absorbers, organic pigments, medicines, fragrances, and insecticides. The method is used for producing dicyclohexyl piperidine, benzatropine hydrobromide, diphenhydramine hydrochloride and the like in the pharmaceutical industry. The product is also styrene polymerization inhibitor and perfume fixing agent. Can impart sweet smell to essence, and can be used in various perfumes and soap essences. Can be used for preparing edible essence such as semen Armeniacae amarum, fructus Persicae, butter, and coconut. It is because of the wide application of benzophenone in life, and its production process is safe and not very small.
Disclosure of Invention
The invention aims at least solving the technical problems in the prior art, and particularly creatively provides a production process of the dimethyl ketone.
In order to achieve the above object, the present invention provides a benzophenone production process comprising the steps of:
s1, firstly, N is introduced 2 A to B times of replacement, wherein A, B is a positive integer of 2 or more and 5 or less, B >A, discharging the replacement waste gas to an alkali sealing tank;
s2, slowly placing the prepared benzene in the benzene metering tank into an photochemical kettle;
s3, slowly adding the prepared aluminum trichloride in the aluminum trichloride charging hopper into an photochemical kettle;
s4, after the addition of benzene and aluminum trichloride is finished, starting an photochemical kettle for stirring;
after stirring and running for a few minutes, if the temperature T of the photochemical kettle is less than or equal to the set temperature, opening jacket steam, and after the temperature of the photochemical kettle is increased to be more than or equal to the set temperature, closing a steam isolation valve on site of the photochemical kettle;
s5, dropwise adding liquid phosgene into an photochemical kettle for photochemical reaction;
s6, slowly filling N into the photochemical kettle 2 After the pressure is built, a discharging valve is slowly opened, and the material is discharged into the hydrolysis kettle;
s7, a hydrolysis process;
s8, a neutralization and water washing process;
s9, a rectification step.
In a preferred embodiment of the present invention, the following steps are included in step S7:
s71, starting a hydrolysis process water pump, starting a manual bypass valve, adjusting the minimum quantity of the water pump, returning the minimum quantity of the water pump to a process water tank, conveying hydrolysis process water to a condenser, reducing the temperature of the process water to a certain temperature when the hydrolysis process water comes out of the condenser, and entering a hydrolysis kettle;
when the water is added into the hydrolysis kettle, starting the hydrolysis kettle for stirring, opening a jacket brine valve of the hydrolysis kettle, cooling the hydrolysis kettle by using frozen brine at the temperature of-15 ℃, and reducing the temperature of the hydrolysis kettle to a certain temperature to prepare for hydrolysis;
S72, when the photochemical kettle enters a discharging step, after the photochemical kettle is ready to discharge, a feeding valve of the hydrolytic kettle is opened, a discharging valve of the photochemical kettle is opened, and the photochemical kettle is slowly pressed into the hydrolytic kettle by nitrogen;
s73, placing the lower-layer aluminum trichloride aqueous solution into an aluminum trichloride aqueous solution cooler, cooling by using water with the temperature of C, wherein C is a positive number less than or equal to 8, controlling the temperature of aluminum salt water within a certain range, then, entering an aluminum trichloride aqueous solution separator for continuous separation, enabling the lower-layer aluminum salt water to enter an aluminum salt water storage tank, and enabling an upper-layer organic phase to automatically flow into a hydrolysis material storage tank;
s74, after the aluminum salt water is discharged, slowly and completely placing the organic phase into a hydrolysis material storage tank; and after the discharging is finished, closing the discharging valve. Returning to step S71.
In a preferred embodiment of the present invention, the following steps are included in step S8:
s81, regulating the flow of D% caustic soda from a tank area through a regulating valve, wherein D is a positive number which is more than or equal to 40 and less than or equal to 60, regulating the flow of fresh water from the outside through the regulating valve, controlling the D% caustic soda and the fresh water to enter a static mixer in a certain proportion, uniformly mixing, preparing E% alkaline water, and entering an alkaline water tank, wherein E is a positive number which is more than or equal to 8 and less than or equal to 12;
S82, conveying the prepared E% alkali liquor to an alkali water elevated tank by using a neutralization alkali liquor pump, after establishing a liquid level in the alkali water elevated tank, overflowing the alkali water from the upper part back to the alkali water tank, opening an alkali water valve from the alkali water elevated tank, putting a small amount of alkali water through a PH value regulating valve, and opening a neutralization kettle for stirring;
s83, after water is discharged from an outlet at the upper part of the neutralization kettle, starting a neutralization feeding pump, controlling the flow through a regulating valve, and feeding hydrolysis materials into the neutralization kettle for neutralization;
after neutralization, the neutralization material automatically flows into a neutralization separator for continuous separation, the lower water phase automatically flows into a hydrolysis process water storage tank for hydrolysis, and the upper organic phase crude benzophenone automatically flows into a first-stage water washing kettle for water washing;
after primary washing, crude benzophenone flows out from the upper part of the primary washing kettle, flows into a primary continuous separator from the upper part for continuous separation, flows out from the upper part, and flows into a secondary washing kettle from the lower part for secondary washing;
after the second-stage water washing, water washing materials flow out from the upper part, flow into the second-stage continuous separator automatically and are continuously separated, flow out from the upper part and flow into a water washing trough automatically for temporary storage;
after entering the secondary washing tank, desalted water sequentially enters the secondary washing tank and the primary washing tank, finally flows into the process tank for hydrolysis and reuse, and after neutralization, also flows into the process tank for production and reuse.
In a preferred embodiment of the present invention, the following steps are included in step S9:
s91, starting a water benzene distillation feed pump, controlling the flow of water washing materials through a regulating valve, sending the water washing materials into a water washing material preheater, preheating the materials by utilizing liquid biphenyl loop biphenyl, controlling the temperature of crude products at an outlet of the preheater, and feeding the crude products into the water benzene distillation tower from the middle upper part of the water benzene distillation tower for normal pressure distillation;
s92, pumping coarse materials into the middle upper part of a light component removal tower by a hydrobenzene distillation extraction pump, and carrying out high-vacuum rectification in the light component removal tower;
s93, continuously extracting the light component removing kettle liquid from the light component removing kettle, entering the rectifying tower kettle, and carrying out high-vacuum rectification in the rectifying tower.
The invention also discloses a safety working system in the benzophenone production process, which comprises an photochemical kettle, wherein a field control panel fixed mounting seat for fixedly mounting a field control panel is arranged on the outer side wall of the photochemical kettle, the field control panel is fixedly mounted on the field control panel fixed mounting seat, an rfid card reader fixed mounting seat for fixedly mounting an rfid card reader, a two-dimensional code identifier fixed mounting seat for fixedly mounting a two-dimensional code identifier and a touch display screen fixed mounting seat for fixedly mounting a touch display screen are arranged on the field control panel, the rfid card reader is fixedly mounted on the rfid card reader fixed mounting seat, the two-dimensional code identifier is fixedly mounted on the two-dimensional code identifier fixed mounting seat, and the touch display screen is fixedly mounted on the touch display screen fixed mounting seat;
The system comprises a field control panel, a network communication module, a field control panel controller, a network data communication end, a rfid card reader, a two-dimensional code identifier, a touch display screen and a field control panel controller, wherein the field control panel controller and the network communication module are arranged on the field control panel;
after the cloud platform receives the safe transmission information sent by the rfid card reader, the cloud platform sends a user code to the intelligent mobile handheld terminal, the rfid card reader displays a terminal two-dimensional code on a display screen of the intelligent mobile handheld terminal after receiving the user code sent by the cloud platform, and the two-dimensional code identifier obtains the terminal two-dimensional code information displayed on the display screen of the intelligent mobile handheld terminal, and after verification, the photochemical kettle starts stirring.
In a preferred embodiment of the present invention, the network communication module comprises a network wired communication module or/and a network wireless communication module;
the wired network data communication end of the field control panel controller is connected with the network data communication end of the network wired communication module, and the wireless network data communication end of the field control panel controller is connected with the network data communication end of the network wireless communication module.
In a preferred embodiment of the present invention, the network wireless communication module includes one or any combination of a 3G network communication module, a 4G network communication module, a 5G network communication module, a WiFi network communication module;
the wireless network data communication 3G end of the field control panel controller is connected with the network data communication end of the 3G network communication module, the wireless network data communication 4G end of the field control panel controller is connected with the network data communication end of the 4G network communication module, the wireless network data communication 5G end of the field control panel controller is connected with the network data communication end of the 5G network communication module, and the wireless network data communication WiFi end of the field control panel controller is connected with the network data communication end of the WiFi network communication module.
In a preferred embodiment of the present invention, the network wired communication module includes one or any combination of a hundred megaweb network communication module, a gigabit network communication module, and an RS485 network communication module;
the wired network data communication hundred megabits end of the field control panel controller is connected with the network data communication end of the hundred megabits network line network communication module, the wired network data communication gigabit end of the field control panel controller is connected with the network data communication end of the gigabit network line network communication module, and the wired network data communication RS485 end of the field control panel controller is connected with the network data communication end of the RS485 network communication module.
The invention also discloses a safe working method in the benzophenone process, which comprises the following steps:
s1, placing a user card at an induction position to enable an rfid card reader to acquire and obtain safety communication information;
s2, after the rfid card reader obtains the safety communication information, obtaining safety transmission information according to the safety communication information;
s3, after the cloud platform obtains the security transmission information, obtaining a user code according to the security transmission information;
s4, after the intelligent mobile handheld terminal obtains the user code, generating a terminal two-dimensional code according to the user code;
s5, the two-dimension code identifier obtains a terminal user code according to the terminal two-dimension code, and the field control panel controller judges whether the terminal user code is consistent with the security decryption information or not:
if the terminal user code is consistent with the safety decryption information, the on-site control panel controller sends a confirmation to start the stirred procedure of the photochemical kettle to the photochemical kettle;
if the end user code is inconsistent with the secure decryption information, the field control panel controller does not send a confirmation to the photochemical kettle to start the photochemical kettle stirring process.
In a preferred embodiment of the present invention, the following steps are included in step S2:
s21, after the rfid card reader receives the secure communication information CommunicationData sent by the user card, decrypting the received secure communication information CommunicationData by using the public key of the user card to obtain decryption information;
S22, converting the decryption information into safe decryption information;
s23, rewriting the security decryption information into security transmission information;
s24, transmitting the safe transmission information SecureTransmit number sixtybinary And transmitting the data to the cloud platform.
In conclusion, by adopting the technical scheme, the invention can safely play a protective role and avoid being attacked.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
fig. 1 is a schematic block diagram of the connection of the present invention.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the invention.
1. Photochemical process
N 2 Replacement: before the photochemical kettle is put into operation, N is introduced 2 And (3) replacing for 2-3 times, discharging the replaced waste gas to an alkali sealing tank, and discharging the waste gas to a high-point of a company emergency treatment system for emptying after the waste gas is captured by an emptying catcher.
When photochemical kettle N 2 And (3) replacing, and putting the vehicle into operation after the driving preparation work is finished. The operation of the photochemical kettle is controlled and supervised by a program.
Step 1, charging
1.1, adding benzene: and slowly placing the prepared benzene in the benzene metering tank into an photochemical kettle, and confirming that the benzene feeding is finished on site.
1.2, adding aluminum trichloride: slowly adding the prepared aluminum trichloride in the aluminum trichloride charging hopper into an photochemical kettle, and confirming that the aluminum trichloride charging is finished on site.
1.3, starting stirring: after the addition of benzene and aluminum trichloride is completed, starting the photochemical kettle for stirring.
After stirring and running for a few minutes (2-3 minutes), if the temperature T of the photochemical kettle is less than or equal to the set temperature, the set temperature is 24-26 ℃, jacket steam is started, after the temperature of the photochemical kettle is increased to be more than or equal to the set temperature, a site steam isolation valve of the photochemical kettle is closed, and steam condensate water and residual steam are discharged to a condensate tank; if the temperature T of the photochemical kettle is more than or equal to the set temperature value, the photochemical step can be carried out.
Step 2: photochemical reaction
When entering the photochemical step, the phosgene flow is regulated by a phosgene flow regulating valve to control the temperature of the photochemical kettle.
The liquid phosgene flows from the condenser discharging pipeline by means of liquid level difference, is monitored by conductivity, and is dripped into the photochemical kettle after being controlled by a photochemical kettle flow regulating valve. The photochemical condensation reflux valve was then opened and photochemical condensation reflux benzene was added.
Photochemical tail gas enters a photochemical tail gas main pipe, and after two-stage condensation, the tail gas enters a hydrogen chloride falling film for absorption. The condensed feed flows into a photochemical reflux continuous separator and is evenly distributed into photochemical kettles in a photochemical step through a reflux benzene main pipe. At the end of the photochemical reaction, the photochemical condensation reflux valve is closed.
During the photochemical process: stirring well; strictly controlling phosgene flow, photochemical temperature and photochemical pressure;
step 3, heating and preserving heat
After the photochemical reaction is finished, a steam regulating valve is opened, the temperature of the photochemical reaction kettle is raised, and the steam condensate is discharged to a condensate tank. The photochemical kettle Wen Yunsu is raised to a certain temperature in a specified time, and the temperature of the photochemical kettle is maintained for a period of time.
In the heating and heat preservation steps, good stirring is kept, the heating speed is strictly controlled, and overtemperature and overpressure are avoided.
Step 4, discharging
Slowly filling N into the photochemical kettle 2 After the pressure is built, a discharging valve is slowly opened, and the material is discharged into the hydrolysis kettle. The discharging speed is controlled by a temperature control valve of the hydrolysis kettle. In the hydrolysis process, the temperature rising speed is controlled, the temperature rising is gentle, and the discharging is finished within a specified time.
After the discharge is finished, confirm N 2 The valve is closed, and after the discharge pipeline is purged by steam, the discharge valve is closed. The residual pressure in the photochemical kettle is discharged to a tail breaking system for treatment through a photochemical condenser.
And (3) returning to the step 1 after the discharge of the photochemical kettle is finished, and feeding.
2. Hydrolysis step
The operation of the hydrolysis kettle adopts program control and supervision. After the photochemical kettle enters stable photochemical, the hydrolysis kettle enters a water preparation step.
Step 1, preparing water
Starting a hydrolysis process water pump, starting a manual bypass valve, returning the lowest limit of the adjusted water pump to a process water tank, conveying the hydrolysis process water to a condenser, reducing the temperature of the process water to a certain temperature when the hydrolysis process water comes out of the condenser, and entering a hydrolysis kettle. When the accumulated water adding amount reaches a set value, the water adding valve is automatically cut off, meanwhile, the flow amount is displayed to return to zero, and the next hydrolysis kettle is prepared for water adding.
When the water is added into the hydrolysis kettle, the hydrolysis kettle is started to stir, a jacket brine valve of the hydrolysis kettle is opened, the hydrolysis kettle is cooled by frozen brine at the temperature of minus 15 ℃, the temperature of the hydrolysis kettle is reduced to a certain temperature, and the hydrolysis kettle is ready to enter hydrolysis.
Step 2, hydrolysis
When the photochemical kettle enters a discharging step, after the photochemical kettle is ready for discharging, a feeding valve of the hydrolytic kettle is opened, a discharging valve of the photochemical kettle is opened, and the photochemical material is slowly pressed into the hydrolytic kettle by nitrogen. Hydrolysis rate: under the condition that the jacket brine of the hydrolysis kettle is fully opened, the temperature of the hydrolysis kettle is controlled by a temperature regulating valve. And the hydrolyzed tail gas enters a first-stage hydrolysis condenser to be condensed, and the condensate flows back to the hydrolysis kettle.
The hydrolyzed tail gas after primary condensation enters a hydrolyzed tail gas main pipe, then enters a secondary hydrolyzed condenser and a tertiary hydrolyzed condenser in sequence, and the noncondensable gas enters a hydrogen chloride falling film for absorption. 2. And the condensate of the three-stage hydrolysis condenser flows into an acid benzene continuous separator for separation.
After a period of time, the photochemical kettle finishes discharging, and after the discharging pipeline is purged, the feeding valve of the hydrolysis kettle is closed.
Step 3, static layering
When the temperature of the hydrolysis kettle is reduced to a certain value, stirring is stopped, cooling is stopped, and materials in the hydrolysis kettle are kept stand for layering.
Step 4, discharging
1.1 placing an aqueous solution of aluminum trichloride
The lower layer of aluminum trichloride aqueous solution is put into an aluminum trichloride aqueous solution cooler, cooled by water at 5 ℃, and the aluminum salt water temperature is controlled within a certain range and then enters an aluminum trichloride aqueous solution separator for continuous separation. The lower aluminum salt water enters an aluminum salt water storage tank, and the upper organic phase automatically flows to a hydrolysis material storage tank.
1.2, discharging and decomposing materials
After the aluminum salt water is discharged, the organic phase is slowly and completely placed into a hydrolysis material storage tank.
And after the discharging is finished, closing the discharging valve. Returning to the step 1, preparing water, and preparing for discharging and hydrolyzing the photochemical kettle.
3. Neutralization and washing process
3.1 alkali Water configuration
The flow rate of 50% caustic soda from a tank area of a company is regulated by a regulating valve, the flow rate of fresh water from the outside is regulated by the regulating valve, the 50% caustic soda and the fresh water are controlled to be mixed uniformly in a static mixer according to a certain proportion, and about 10% of alkaline water is prepared and enters an alkaline water tank. Controlling the liquid level of the alkaline water tank. And (3) starting heating steam, and controlling the temperature of the alkali liquor within a certain range.
3.2 neutralizing and washing with water
And (3) conveying the prepared 10% alkali liquor to an alkali liquor high-level tank by using a neutralizing alkali liquor pump, and overflowing the alkali liquor high-level tank from the upper part to return the alkali liquor tank after establishing the liquid level. And opening an alkaline water valve from an alkaline water high-level tank, putting a small amount of alkaline water into the alkaline water tank through a PH value regulating valve, and opening a neutralization kettle for stirring.
After water is discharged from an outlet at the upper part of the neutralization kettle, a neutralization feeding pump is started, the flow is controlled through a regulating valve, and hydrolysis materials are fed into the neutralization kettle for neutralization. Controlling the PH value of the outlet to be 10-12.
After neutralization, the neutralization material automatically flows into a neutralization separator for continuous separation, the lower water phase automatically flows into a hydrolysis process water storage tank for hydrolysis, and the upper organic phase crude benzophenone automatically flows into a first-stage water washing kettle for water washing.
After primary washing, crude benzophenone flows out from the upper part of the primary washing kettle, flows into the primary continuous separator from the upper part for continuous separation, flows out from the upper part, and flows into the secondary washing kettle from the lower part for secondary washing.
After the second-stage water washing, water washing materials flow out from the upper part, flow into the second-stage continuous separator to be continuously separated, flow out from the upper part, and flow into a water washing trough for temporary storage.
After entering the secondary washing tank, desalted water sequentially enters the secondary washing tank and the primary washing tank, and finally flows into the process water tank for hydrolysis and reuse. And (3) neutralizing and supplementing water, and flowing into a process water tank for production and application after neutralization.
After a period of operation, sampling and checking each separator (a neutralization separator, a first-stage water washing separator and a second-stage water washing separator) to observe the accumulation state of suspended matters, and if the suspended matters are too many, driving the suspended matters into a suspended matter treatment tank by adding water for centralized treatment. Recovering benzene and other useful materials in the suspended matters.
The neutralization and water washing processes are strictly controlled by the neutralization feeding amount, the PH value of the outlet of the neutralization kettle, the proportion of the neutralization feeding to the neutralization feeding water and the proportion of the neutralization feeding to the water washing soft water; the balance of the liquid level of the primary water washing tank, the secondary water washing tank and the neutralization water tank is regulated; according to photochemical and hydrolytic loads, the neutralization and water washing loads are regulated in a balanced mode, and the phenomenon that the water washing material storage tank is too low in liquid level, too high in liquid level or full in tank is avoided.
4. Rectification process
4.1, water benzene distillation
When the rectifying system finishes the operation preparation work and the liquid level in the water washing tank reaches 50%, the water benzene distillation is put into operation.
Starting a water benzene distillation feed pump, controlling the flow of water washing materials through a regulating valve, sending the water washing materials into a water washing material preheater, preheating the materials by utilizing liquid biphenyl loop biphenyl, controlling the temperature of crude products at an outlet of the preheater, and feeding the crude products into the water benzene distillation tower from the middle upper part of the water benzene distillation tower for normal pressure distillation.
The liquid phase flows into the tower kettle and then enters a water benzene reboiler, water vapor is adopted to heat materials, and the temperature of the tower kettle is controlled. Controlling the liquid level in the tower kettle, pumping out (controlling benzene content less than or equal to 6%) and feeding the liquid to the middle upper part of the dehydrogenation tower.
The reboiler at the tower kettle takes water vapor as a heating medium, and the water vapor is subjected to flash evaporation by a low-pressure flash tank after heat exchange.
The gas phase is condensed and reflowed by a built-in condenser at the top of the tower, the temperature of the top of the tower is controlled, the gas phase is extracted from the top of the tower and sequentially enters a first-stage condenser, a second-stage condenser and a third-stage condenser for condensation, and the non-condensable gas enters an emptying catcher for trapping.
The built-in condenser and the primary condenser use circulating cooling water as cooling medium; the secondary condenser and the tertiary condenser use water with the temperature of 5 ℃ as cooling medium.
And after the condensation and blanking of each stage at the top of the tower are converged, the condensate and blanking enter a water-benzene separator for continuous water separation. The water phase enters a secondary water washing tank for water washing. The organic phase enters a benzene recovery tank for recycling.
In the operation of the hydrobenzene distillation system, the feeding amount, the feeding temperature, the tower top temperature, the tower bottom liquid level and the tower internal pressure need to be strictly controlled.
4.2, light weight removal
The crude material is pumped into the middle upper part of the light component removing tower by the water benzene distillation extraction pump, and high vacuum rectification is carried out in the light component removing tower. Controlling the pressure at the top of the tower, the pressure at the bottom of the tower and the reflux ratio.
After flowing into the light component removing tower, the liquid phase material is pumped into a reboiler for forced circulation heating through a light component removing forced circulation pump, and the temperature of the tower is controlled. And controlling the liquid level of the tower kettle, continuously extracting crude benzophenone with low boiling point substance content less than 0.05% and benzene trace amount, and feeding the crude benzophenone into the rectifying tower kettle for rectification.
The reboiler at the tower kettle takes biphenyl steam as a heating medium, and after heat exchange, biphenyl ether condensate liquid enters a biphenyl condensate liquid reflux main pipe.
The gas phase is condensed and reflowed through a light component removing built-in condenser, the temperature of the top of the tower is controlled to be in a range from the top of the tower, after entering a primary light component removing condenser and a secondary light component removing condenser in sequence, non-condensable gas enters a light component removing vacuum buffer tank to be trapped, and is pumped through a Roots water ring vacuum unit, condensed and trapped, and discharged to a high point of an emergency system of a company to be discharged.
The secondary light component removing condenser condenses the discharged self-flowing backwater washing material storage tank. After a period of operation, sampling and checking, and if the light fraction content exceeds about 3.8%, placing the light fraction into a light fraction removal receiving tank; and when the light fraction content is less than 2%, the water is returned to the water washing tank. When 80% of the light fraction is accumulated in the light fraction removing receiving tank, the light fraction is put into a residual liquid distillation kettle for recovery treatment.
In the operation of the light component removing system, the vacuum, the tower top temperature, the tower bottom liquid level and the alkali adding amount are required to be strictly controlled; the forced circulation of the tower kettle is required to be kept good; the condensed feed needs to be analyzed periodically to avoid accumulation of low-boiling-point substances.
4.3, rectifying
Continuously extracting light component removing liquid from the light component removing tower kettle, wherein the content of low-boiling components is less than 0.05%, the content of high-boiling components is less than 0.5%, the content of alkali salt is less than 0.2%, and feeding the light component removing liquid into the rectifying tower kettle, and carrying out high-vacuum rectification in the rectifying tower.
And pumping tower kettle materials into a reboiler through a slurry pump to perform forced circulation heating, and controlling the temperature of the tower kettle.
And (3) enabling gas-phase materials to come out of the top of the rectifying tower, sequentially entering a primary rectifying condenser and a secondary rectifying condenser for condensation, enabling non-condensable gas to enter a rectifying vacuum buffer tank for collection, sucking through a Roots water ring vacuum unit, collecting again after condensation, and discharging to a high point of an emergency system of a company for emptying.
1. And (3) discharging by secondary rectification condensation, flowing into a rectification reflux tank, pumping out materials by adopting a rectification reflux pump, refluxing one strand to the top of the rectification tower, adjusting the other strand of finished products to be extracted, and controlling the liquid level and reflux ratio of the reflux tank. And periodically sampling and analyzing at the outlet of the reflux pump, and timely adjusting the operation parameters to produce qualified products.
And (5) extracting the finished product into a benzophenone finished product tank, and receiving one for later use. And switching when the liquid level of the finished product tank reaches 80%. After sampling analysis is qualified, N is utilized 2 And (5) conveying the finished product to a solid package for packaging.
And continuously extracting the kettle liquid into a residual liquid collecting tank or a residual liquid distillation kettle by utilizing a residual liquid extracting pump so as to control the content of high-boiling substances and the content of alkali salts in the kettle.
The reboiler at the tower kettle adopts vaporous diphenyl ether as a heating medium, and after heat exchange, biphenyl ether condensate enters a biphenyl condensate reflux main pipe.
In the operation of the rectification system, the vacuum, the reflux quantity of the tower top, the temperature of the tower bottom, the liquid level of the tower bottom, the residual liquid extraction quantity and the liquid level of a reflux tank are required to be strictly controlled; the forced circulation of the tower kettle is required to be kept good; periodic sampling analysis is needed to ensure that a qualified product is produced.
The invention also discloses a safety working system in the benzophenone production process, which comprises an photochemical kettle, wherein a field control panel fixed mounting seat for fixedly mounting a field control panel is arranged on the outer side wall of the photochemical kettle, the field control panel is fixedly mounted on the field control panel fixed mounting seat, an rfid card reader fixed mounting seat for fixedly mounting an rfid card reader, a two-dimensional code identifier fixed mounting seat for fixedly mounting a two-dimensional code identifier and a touch display screen fixed mounting seat for fixedly mounting a touch display screen are arranged on the field control panel, the rfid card reader is fixedly mounted on the rfid card reader fixed mounting seat, the two-dimensional code identifier is fixedly mounted on the two-dimensional code identifier fixed mounting seat, and the touch display screen is fixedly mounted on the touch display screen fixed mounting seat;
The system comprises a field control panel, a network communication module, a field control panel controller, a network data communication end, a rfid card reader, a two-dimensional code identifier, a touch display screen and a field control panel controller, wherein the field control panel controller and the network communication module are arranged on the field control panel;
after the cloud platform receives the safe transmission information sent by the rfid card reader, the cloud platform sends a user code to the intelligent mobile handheld terminal, the rfid card reader displays a terminal two-dimensional code on a display screen of the intelligent mobile handheld terminal after receiving the user code sent by the cloud platform, and the two-dimensional code identifier obtains the terminal two-dimensional code information displayed on the display screen of the intelligent mobile handheld terminal, and after verification, the photochemical kettle starts stirring.
In a preferred embodiment of the present invention, the network communication module comprises a network wired communication module or/and a network wireless communication module;
the wired network data communication end of the field control panel controller is connected with the network data communication end of the network wired communication module, and the wireless network data communication end of the field control panel controller is connected with the network data communication end of the network wireless communication module.
In a preferred embodiment of the present invention, the network wireless communication module includes one or any combination of a 3G network communication module, a 4G network communication module, a 5G network communication module, a WiFi network communication module;
the wireless network data communication 3G end of the field control panel controller is connected with the network data communication end of the 3G network communication module, the wireless network data communication 4G end of the field control panel controller is connected with the network data communication end of the 4G network communication module, the wireless network data communication 5G end of the field control panel controller is connected with the network data communication end of the 5G network communication module, and the wireless network data communication WiFi end of the field control panel controller is connected with the network data communication end of the WiFi network communication module;
the network wired communication module comprises one or any combination of a hundred mega network line network communication module, a gigamega network line network communication module and an RS485 network communication module;
the wired network data communication hundred megabits end of the field control panel controller is connected with the network data communication end of the hundred megabits network line network communication module, the wired network data communication gigabit end of the field control panel controller is connected with the network data communication end of the gigabit network line network communication module, and the wired network data communication RS485 end of the field control panel controller is connected with the network data communication end of the RS485 network communication module.
The invention also discloses a safe working method in the benzophenone process, which comprises the following steps:
s1, placing a user card at an induction position to enable an rfid card reader to acquire and obtain safety communication information;
s2, after the rfid card reader obtains the safety communication information, obtaining safety transmission information according to the safety communication information;
s3, after the cloud platform obtains the security transmission information, obtaining a user code according to the security transmission information;
s4, after the intelligent mobile handheld terminal obtains the user code, generating a terminal two-dimensional code according to the user code;
s5, the two-dimension code identifier obtains a terminal user code according to the terminal two-dimension code, and the field control panel controller judges whether the terminal user code is consistent with the security decryption information or not:
if the terminal user code is consistent with the security decryption information, the user card has relevance with the terminal two-dimensional code displayed on the intelligent mobile handheld terminal, and the on-site control panel controller sends a confirmation to start the stirred procedure of the photochemical kettle to the photochemical kettle;
if the terminal user code is inconsistent with the safety decryption information, the user card is not associated with the terminal two-dimensional code displayed on the intelligent mobile handheld terminal, and the on-site control panel controller does not send a confirmation to start the stirred process of the photochemical kettle to the photochemical kettle.
In a preferred embodiment of the present invention, the following steps are included in step S1:
s11, establishing communication between the user card and the rfid card reader, and executing the next step after the communication between the user card and the rfid card reader is established;
s12, the user card transmits the user card public key to the rfid card reader, and the rfid card reader judges whether the user card public key sent by the user card is received or not:
if the rfid card reader receives the user card public key sent by the user card, executing the next step;
if the rfid reader does not receive the user card public key sent by the user card, returning to the step S12;
s13, after the rfid card reader receives the user card public key sent by the user card, the rfid card reader transmits the cloud platform public key to the user card, and the user card judges whether the cloud platform public key sent by the rfid card reader is received or not:
if the user card receives the cloud platform public key sent by the rfid card reader, executing the next step;
if the user card does not receive the cloud platform public key sent by the rfid card reader, returning to the step S13;
s14, after the user card receives the cloud platform public key sent by the rfid card reader, the user card acquires the security information stored in the user card, and the security communication information is obtained by utilizing the cloud platform public key and the user card private key according to the acquired security information; the method for obtaining the secure communication information by utilizing the cloud platform public key and the user card private key according to the obtained secure information comprises the following steps:
S141, decrypting the security information by using the cloud platform public key to obtain original information, wherein the calculation expression is as follows:
RealData＝Asymmetric decryption algorithm(SecurityData,Cloudplatform PK)，
wherein RealData represents original information;
asymmetric decryption algorithm (,) represents an asymmetric decryption function;
SecurityData represents security information;
cloudplatform PK represents cloud platform public key;
the method for writing the security information into the user card comprises the following steps:
in the first step, the cloud platform obtains the original information to be written into the user card, where the original information is not limited to the ID strings defined by the user, such as admin123, user001, password33, etc., but may also be the data information of the user, such as name, identification card number, mobile phone number, etc. The cloud platform safe transmission information is bound with the account number logged in on the corresponding intelligent mobile handheld terminal.
Secondly, encrypting the original information by using a platform private key to obtain the security information of the user card to be written, wherein the security information is calculated as follows:
CommunicationData″＝Asymmetric encryption algorithm(RealData,Cloudplatform SK)，
wherein CommunicationData "represents security information to be written into the user card;
asymmetric encryption algorithm (,) represents an asymmetric encryption function; the asymmetric encryption function and the asymmetric decryption function are asymmetric algorithms, and RSA and ECDSA can be adopted.
RealData represents original information;
cloudplatform SK represents a cloud platform private key;
and thirdly, writing the security information CommunicationData' to be written into the user card.
S142, encrypting the original information by using a user card private key to obtain safe communication information, wherein the calculation expression is as follows:
CommunicationData＝Asymmetric encryption algorithm(RealData,Usercard SK)，
wherein CommunicationData represents secure communication information;
asymmetric encryption algorithm (,) represents an asymmetric encryption function;
RealData represents original information;
usercard SK represents a user card private key;
s15, the user card transmits the secure communication information CommunicationData to the rfid card reader.
In a preferred embodiment of the present invention, the following steps are included in step S2:
s21, after the rfid card reader receives the secure communication information communication data sent by the user card, decrypting the received secure communication information communication data by using the public key of the user card to obtain decryption information, wherein the calculation expression is as follows:
RealData′＝Asymmetric decryption algorithm(SecurityData′,Usercard PK)，
wherein RealData' represents decryption information;
asymmetric decryption algorithm (,) represents an asymmetric decryption function;
SecurityData' represents the secure communication information CommunicationData received by the rfid reader;
usercard PK represents a user card public key;
S22, converting the decryption information into safe decryption information, wherein the calculation expression is as follows:
RealData″＝One-way math functions(RealData′)，
RealData "represents secure decryption information; the secure decryption information is a sixteen-bit thirty-binary or thirty-two-bit thirty-binary string; the corresponding numerical values are as follows:
one-way math functions () represents a One-way hash algorithm, typically taking the MD5 hash algorithm;
RealData' represents decryption information;
s23, rewriting the security decryption information into the security transmission information, and rewriting the security decryption information into the security transmission information, wherein the method comprises the following steps:
s231, judging whether the safety transmission information is sixty binary:
if the security transmission information is sixty binary values, then securemsstionnumber=securemsstionnumber sixtybinary The method comprises the steps of carrying out a first treatment on the surface of the Wherein SecureTransmit Number represents secure transmission information sixtybinary Representing sixty binary secure transmission information; step S24 is executed;
if the security transmission information security number is not sixty binary values, the security transmission information security number is converted into sixty binary security transmission information, and the method for converting the security transmission information security number into sixty binary security transmission information is as follows:
S2311, converting the secure transmission information secure transmission number into a decimal value, and converting the secure transmission information secure transmission number into a decimal value comprises the following steps:
wherein, the SecureTransmit Number decimal Secure transmission information representing decimal;
s represents the total number of bits of the secure transmission information secure number;
S i representing a value corresponding to an ith bit in the sequence from the lowest bit to the highest bit of the secure transmission information SecureTransmit number;
<S> i-1 representation of<S>I-1 th power of (2);
< S > represents a binary value corresponding to the secure transmission information secure number;
s2312, security transmission information security number of decimal system decimal Secure transmission information securtransmissionnumber converted into sixty binary system sixtybinary The decimal security transmission information is securransmission number decimal Secure transmission information securtransmissionnumber converted into sixty binary system sixtybinary The method of (1) is as follows:
s23121, let iteration first self-increment a=1; a is that 1 ＝SecuretransmissionNumber decimal ；
S23122，
Wherein A is a+1 Representing a +1th iteration result value;
int|| represents a rounding down operation;
A a representing a th iteration result value;
judgment A a+1 Size relationship with 0, 61 and 62:
if A a+1 Not less than 62, a=a+1, returning to step S23122;
If 0 is less than or equal to A a+1 Less than or equal to 61, the following steps S231221-S231222 are executed;
s231221, let iteration second self-increment b=1;
S231222，B b ＝A b mod62，
wherein mod represents a remainder operation;
A b representing a b-th iteration result value;
B b representing the b-th result value;
judging the relation between b and a:
if a+.b, b=b+1, returning to S22132;
if a=b, then SecuretransposionNumber sixtybinary ＝B a B a-1 B a-2 …B 3 B 2 B 1 The method comprises the steps of carrying out a first treatment on the surface of the Step S24 is executed;
wherein, the SecureTransmit Number sixtybinary Secure transmission information representing sixty-binary;
B a representing the a-th result value;
B a-1 representing the a-1 th result value;
B a-2 representing the a-2 th result value;
B 3 representing the 3 rd result value;
B 2 representing the 2 nd result value;
B 1 the 1 st result value is shown.
S24, transmitting the safe transmission information SecureTransmit number sixtybinary And transmitting the data to the cloud platform.
In a preferred embodiment of the present invention, the following steps are included in step S3:
s31, the received security transmission information security number sixtybinary Converting into decimal value, and transmitting the received safe transmission information security number sixtybinary The method for converting the decimal value comprises the following steps:
wherein, the SecureTransmit Number d ′ ecimal The decimal cloud platform safety transmission information is represented;
the S' indicates the received secure transmission information secure number sixtybinary Is a total number of bits of (2);
S′ i representing the received security transmission information security number sixtybinary The value corresponding to the ith bit in the sequence from the lowest bit to the highest bit;
62 i-1 i-1 th power of the representation 62;
s32, transmitting information security number 'of decimal cloud platform' decimal Converting into security transmission information with the same system as the security transmission information security number in step S231, and security transmission information security number of decimal cloud platform d ′ ecimal The method for converting to the same security transmission information as the security transmission information number in step S231 is as follows:
s321, let iteration third self-increment a' =1; a is that 1 ′＝SecuretransmissionNumber d ′ ecimal ；
S322，
Wherein A 'is' a′+1 Representing a (a' +1) th iteration cloud platform result value;
int|| represents a rounding down operation;
< S > represents a binary value of secure transmission information secure number;
A′ a′ representing a result value of the a-th iteration cloud platform;
judging A' a′+1 Size relationship with 0, 61 and 62:
if A' a′+1 Gtoreq 62, a '=a' +1, return to step S322;
if 0 is less than or equal to A' a′+1 If not more than 61, the following steps S3221 to S3222 are executed;
s3221, let iteration fourth self-increment number b' =1;
S3222，B′ b′ ＝A′ b′ mod<S>，
wherein mod represents a remainder operation;
A′ b′ representing a b' th iteration cloud platform result value;
B′ b′ Representing the b' th cloud platform junctionFruit value;
< S > represents a binary value of secure transmission information secure number;
judging the relation between b 'and a':
if a '+.b', b '=b' +1, return to S3222;
if a '=b', then securranspossessionnumber '=b' a′ B′ a′-1 B′ a′-2 …B′ 3 B′ 2 B′ 1 The method comprises the steps of carrying out a first treatment on the surface of the Step S33 is performed; the secure transmissionnumber' represents secure transmission information of the cloud platform;
B′ a′ representing a' cloud platform result value;
B′ a′-1 representing a' -1 cloud platform result value;
B′ a′-2 representing a' -2 cloud platform result value;
B′ 3 representing a 3 rd cloud platform result value;
B′ 2 representing a result value of the 2 nd cloud platform;
B′ 1 and representing the result value of the 1 st cloud platform.
S33, converting the cloud platform security transmission information SecureTransmit number' into a two-dimensional code image; sequentially extracting numerical values according to the colors of all the squares in the two-dimensional code image from left to right and from top to bottom to obtain a 0-1 character string; the method for obtaining the numerical value according to the color of the square lattice in the two-dimensional code image comprises the following steps:
where if represents a logical conditional if;
D d,d′ =black square means that the color of the d' th square of the d-th row is black; d=1, 2, 3, … …, d ", d' =1, 2, 3, … …, d",d' "represents the total number of squares in the two-dimensional code image, and d" represents the two-dimensional code The total number of square grids in each row or each column in the image; if d>62, d "=62;
D d,d′ =white represents that the color of the d' th square of the d row is white;
E d,d′ a numerical value representing the color of the d' th square of the d-th row;
s34, converting the 0-1 character string into a d 'character string, and converting the 0-1 character string into the d' character string by the following steps:
s341, converting the binary 0-1 character string into a decimal value, and converting the binary 0-1 character string into the decimal value by the following steps:
wherein, secureTransmit Number decimal A character string representing decimal system;
the S represents the total number of bits of the 0-1 string;
S″ i representing the value corresponding to the ith bit in the sequence from the lowest bit to the highest bit of the 0-1 character string;
2 i-1 i-1 th power of 2;
s342, the decimal character string SecureTransmit Number decimal Converting the character string into a d 'system character string, wherein the d' system character string is the user code; the decimal character string SecureTransmit Number decimal The method for converting the character string into d' system is as follows:
s3421, let iteration fifth self-increment a "=1; a' 1 ＝SecuretransmissionNumber″ decimal ；
S3422，
Wherein A' a″+1 Representing a "+1-th iteration image result value;
int|| represents a rounding down operation;
d' represents the total number of square grids in each row or each column in the two-dimensional code image;
A″ a″ Representing a "th" iteration image result value;
judging A a″+1 Size relationship with 0, d ", and d" -1:
if A a″+1 Gtoreq d ", a" =a "+1, returning to step S3422;
if 0 is less than or equal to A% a″+1 D' -1, executing the following steps S34221-S34222;
s34221, let iteration sixth self-increment b "=1;
S34222，B″ b″ ＝A″ b″ modd″，
wherein mod represents a remainder operation;
A″ b″ representing the b "th iteration image result value;
B″ b″ representing the b "th image result value;
d' represents the total number of square grids in each row or each column in the two-dimensional code image;
judging the relation between b 'and a':
if a "is not equal to b", b "=b" +1, return to S34222;
if a "=b", then securemssionnumber "=b" a″ B″ a″-1 B″ a″-2 …B″ 3 B″ 2 B″ 1 The method comprises the steps of carrying out a first treatment on the surface of the Step S35 is performed;
wherein, the SecureTransmit number represents a character string of d' system;
B″ a″ representing an a "th image result value;
B″ a″-1 representing an a "-1 th image result value;
B″ a″-2 representing an a "-2 th image result value;
B″ 3 representing the 3 rd image result value;
B″ 2 representing the 2 nd image result value;
B″ 1 representing the 1 st image result value;
and S35, the user code is sent to the intelligent mobile handheld terminal.
In a preferred embodiment of the present invention, the following steps are included in step S4:
s41, converting the received user code SecureTransmit Number 'into a decimal value, wherein the method for converting the received user code SecureTransmit Number' into the decimal value comprises the following steps:
Wherein, the SecureTransmit Number d ″′ ecimal A user code representing decimal;
the S '"represents the total number of bits of the received user code securtransmissionnumber'";
S″′ i representing the value corresponding to the ith bit in the sequence from the lowest bit to the highest bit of the received user code SecureTransmisionNumber';
d″ i-1 represents the power of i-1 of d';
d' represents the total number of squares in each row or column in the two-dimensional code image in step S33;
s42, decimal user code SecureTransmit Number' decimal Converting into binary user code, and transmitting decimal user code' decimal The method for converting the user code into the binary system comprises the following steps:
s421, let iteration seventh self-increment a' "=1; a'. 1 ＝SecuretransmissionNumber″′ decimal ；
S422，
Wherein A' a″+1 Representing a final value of the a' +1 iteration;
int|| represents a rounding down operation;
A″′ a″ representing an a' "th iteration terminal result value;
judging A '' a″+1 Size relationship with 0, 2 and 1:
if A' a′+1 Gtoreq 2, a '"=a'" +1, returning to step S422;
if 0 is less than or equal to A '' a″+1 If the temperature is less than or equal to 1, the following steps S4221 to S4222 are executed;
s4221, let iteration eighth self-increment b' "=1;
S4222，B″′ b″ ＝A″′b ″ mod2，
wherein mod represents a remainder operation;
A″′ b″ representing a b' "th iteration terminal result value;
B″′ b″ Representing a b' "th terminal result value;
judging the relation between b '"and a'" of the formula:
if a '"is not equal to b'", b '"=b'" +1, returning to S4222;
if a ' "=b '", then securemssionnumber ' "=b '" ' a″′ B″′ a″′-1 B″′ a″′-2 …B″′ 3 B″′ 2 B″′ 1 The method comprises the steps of carrying out a first treatment on the surface of the Step S43 is performed;
wherein, the SecureTransmit number' "represents a binary terminal character string;
B″′ a″′ representing an a' "th terminal result value;
B″′ a″′-1 representing the a' -1 th terminal result value;
B″′ a″′-2 representing an a' -2 th terminal result value;
B″′ 3 representing a 3 rd terminal result value;
B″′ 2 representing the result value of the 2 nd terminal;
B″′ 1 the 1 st terminal result value is shown.
S43, generating a table of d ' squares and d ' squares in each row, sequentially filling binary terminal character strings SecureTransmit Number ' into the squares in the order from left to right and from top to bottom, if the squares are filled with 1, the squares are whitened, if the squares are filled with 0, the squares are darkened, and the table grid lines are removed, so that the terminal two-dimensional code is obtained.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: many changes, modifications, substitutions and variations may be made to the embodiments without departing from the spirit and principles of the invention, the scope of which is defined by the claims and their equivalents.
Claims (1)
1. The benzophenone production process is characterized by comprising the following steps of:
s1, firstly, N is introduced 2 A to B times of replacement, wherein A, B is a positive integer of 2 or more and 5 or less, B>A, discharging the replacement waste gas to an alkali sealing tank;
s2, slowly placing the prepared benzene in the benzene metering tank into an photochemical kettle;
s3, slowly adding the prepared aluminum trichloride in the aluminum trichloride charging hopper into an photochemical kettle;
s4, after the addition of benzene and aluminum trichloride is finished, starting an photochemical kettle for stirring;
after stirring and running for a few minutes, if the temperature T of the photochemical kettle is less than or equal to the set temperature, opening jacket steam, and after the temperature of the photochemical kettle is increased to be more than or equal to the set temperature, closing a steam isolation valve on site of the photochemical kettle;
s5, dropwise adding liquid phosgene into an photochemical kettle for photochemical reaction;
s6, slowly filling N into the photochemical kettle 2 After the pressure is built, a discharging valve is slowly opened, and the material is discharged into the hydrolysis kettle;
s7, a hydrolysis process; the hydrolysis process comprises the following steps:
s71, starting a hydrolysis process water pump, starting a manual bypass valve, adjusting the minimum quantity of the water pump, returning the minimum quantity of the water pump to a process water tank, conveying hydrolysis process water to a condenser, reducing the temperature of the process water to a certain temperature when the hydrolysis process water comes out of the condenser, and entering a hydrolysis kettle;
When the water is added into the hydrolysis kettle, starting the hydrolysis kettle for stirring, opening a jacket brine valve of the hydrolysis kettle, cooling the hydrolysis kettle by using frozen brine at the temperature of-15 ℃, and reducing the temperature of the hydrolysis kettle to a certain temperature to prepare for hydrolysis;
s72, when the photochemical kettle enters a discharging step, after the photochemical kettle is ready to discharge, a feeding valve of the hydrolytic kettle is opened, a discharging valve of the photochemical kettle is opened, and the photochemical kettle is slowly pressed into the hydrolytic kettle by nitrogen;
s73, placing the lower-layer aluminum trichloride aqueous solution into an aluminum trichloride aqueous solution cooler, cooling by using water with the temperature of C, wherein C is a positive number less than or equal to 8, controlling the temperature of aluminum salt water within a certain range, then, entering an aluminum trichloride aqueous solution separator for continuous separation, enabling the lower-layer aluminum salt water to enter an aluminum salt water storage tank, and enabling an upper-layer organic phase to automatically flow into a hydrolysis material storage tank;
s74, after the aluminum salt water is discharged, slowly and completely placing the organic phase into a hydrolysis material storage tank; after the discharging is finished, closing a discharging valve, and returning to the step S71;
s8, a neutralization and water washing process; wherein the neutralization and water washing procedures comprise the following steps:
s81, regulating the flow of D% caustic soda from a tank area through a regulating valve, wherein D is a positive number which is more than or equal to 40 and less than or equal to 60, regulating the flow of fresh water from the outside through the regulating valve, controlling the D% caustic soda and the fresh water to enter a static mixer in a certain proportion, uniformly mixing, preparing E% alkaline water, and entering an alkaline water tank, wherein E is a positive number which is more than or equal to 8 and less than or equal to 12;
S82, conveying the prepared E% alkali liquor to an alkali water elevated tank by using a neutralization alkali liquor pump, after establishing a liquid level in the alkali water elevated tank, overflowing the alkali water from the upper part back to the alkali water tank, opening an alkali water valve from the alkali water elevated tank, putting a small amount of alkali water through a PH value regulating valve, and opening a neutralization kettle for stirring;
s83, after water is discharged from an outlet at the upper part of the neutralization kettle, starting a neutralization feeding pump, controlling the flow through a regulating valve, and feeding hydrolysis materials into the neutralization kettle for neutralization;
after neutralization, the neutralization material automatically flows into a neutralization separator for continuous separation, the lower water phase automatically flows into a hydrolysis process water storage tank for hydrolysis, and the upper organic phase crude benzophenone automatically flows into a first-stage water washing kettle for water washing;
after primary washing, crude benzophenone flows out from the upper part of the primary washing kettle, flows into a primary continuous separator from the upper part for continuous separation, flows out from the upper part, and flows into a secondary washing kettle from the lower part for secondary washing;
after the second-stage water washing, water washing materials flow out from the upper part, flow into the second-stage continuous separator automatically and are continuously separated, flow out from the upper part and flow into a water washing trough automatically for temporary storage;
after entering the secondary washing tank, desalted water sequentially enters the secondary washing tank and the primary washing tank, finally flows into the process tank for hydrolysis and reuse, and after neutralization, also flows into the process tank for production and reuse;
S9, a rectification process, wherein the rectification process comprises the following steps of:
s91, starting a water benzene distillation feed pump, controlling the flow of water washing materials through a regulating valve, sending the water washing materials into a water washing material preheater, preheating the materials by utilizing liquid biphenyl loop biphenyl, controlling the temperature of crude products at an outlet of the preheater, and feeding the crude products into the water benzene distillation tower from the middle upper part of the water benzene distillation tower for normal pressure distillation;
s92, pumping coarse materials into the middle upper part of a light component removal tower by a hydrobenzene distillation extraction pump, and carrying out high-vacuum rectification in the light component removal tower;
s93, continuously extracting a light component removing kettle liquid from the light component removing kettle, feeding the light component removing kettle liquid into a rectifying tower kettle, and carrying out high-vacuum rectification in the rectifying tower;
the photochemical kettle is as follows: the method comprises the steps that a field control panel fixed mounting seat for fixedly mounting a field control panel is arranged on the outer side wall of an photochemical kettle body, the field control panel is fixedly mounted on the field control panel fixed mounting seat, an rfid card reader fixed mounting seat for fixedly mounting an rfid card reader, a two-dimensional code identifier fixed mounting seat for fixedly mounting a two-dimensional code identifier and a touch display screen fixed mounting seat for fixedly mounting a touch display screen are arranged on the field control panel, the rfid card reader is fixedly mounted on the rfid card reader fixed mounting seat, the two-dimensional code identifier is fixedly mounted on the two-dimensional code identifier fixed mounting seat, and the touch display screen is fixedly mounted on the touch display screen fixed mounting seat;
The system also comprises a field control panel controller and a network communication module which are arranged on the field control panel, wherein the network communication module comprises a network wired communication module or/and a network wireless communication module;
the network wireless communication module comprises one or any combination of a 3G network communication module, a 4G network communication module, a 5G network communication module and a WiFi network communication module; the wireless network data communication 3G end of the field control panel controller is connected with the network data communication end of the 3G network communication module, the wireless network data communication 4G end of the field control panel controller is connected with the network data communication end of the 4G network communication module, the wireless network data communication 5G end of the field control panel controller is connected with the network data communication end of the 5G network communication module, and the wireless network data communication WiFi end of the field control panel controller is connected with the network data communication end of the WiFi network communication module;
the network wired communication module comprises one or any combination of a hundred mega network line network communication module, a gigamega network line network communication module and an RS485 network communication module; the wired network data communication hundred megabits end of the field control panel controller is connected with the network data communication end of the hundred megabits network line network communication module, the wired network data communication gigabit end of the field control panel controller is connected with the network data communication end of the gigabit network line network communication module, and the wired network data communication RS485 end of the field control panel controller is connected with the network data communication end of the RS485 network communication module;
The data reading output end of the rfid card reader is connected with the data reading input end of the field control panel controller, the data identification output end of the two-dimensional code identifier is connected with the data identification input end of the field control panel controller, and the data touch display end of the touch display screen is connected with the data touch display end of the field control panel controller;
after the cloud platform receives the safe transmission information sent by the rfid card reader, the cloud platform sends a user code to the intelligent mobile handheld terminal, the rfid card reader displays a terminal two-dimensional code on a display screen of the intelligent mobile handheld terminal after receiving the user code sent by the cloud platform, and the two-dimensional code identifier obtains the terminal two-dimensional code information displayed on the display screen of the intelligent mobile handheld terminal, and after verification, the photochemical kettle starts stirring.
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