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The diazotization process is prone to decomposition, generating pressure that can cause the reaction vessel to explode; it is therefore classified as a high-risk process. In the factory, diazotization is carried out in large uncovered wooden barrels filled with a large amount of ice; no heating is used, so there is no temperature (it remains around 0 degrees, and since there is plenty of ice, temperature measurement isn’t necessary). There is also no pressure, and decomposition due to uncontrolled temperature does not result in any pressure buildup (even if decomposition occurs in an open barrel, no pressure is generated). Such equipment also falls under the category of high-risk process equipment – should it be automated?
Is the reaction carried out in a wooden barrel?
Thank you to the original poster for their vivid imagination; I’ve learned something new. ;P
Jiangsu Provincial Work Safety Supervision Bureau (Opinions) Su An Jian [2009] No. 109 ________________________________________ Opinions on Standardizing the Technical Upgrades Related to Automatic Control in Chemical Enterprises To the work safety supervision bureaus of various cities: In order to accelerate the advancement of automatic control in chemical production processes, gradually achieve intrinsic safety in chemical enterprises, and effectively prevent accidents involving hazardous chemicals, in accordance with the requirements of the Work Safety Law, the Regulations on Work Safety Licenses, the Guidelines issued by the Office of the State Council’s Work Safety Committee on Further Strengthening Work Safety in the Handling of Hazardous Chemicals, and the Notice from the Provincial ** Office forwarding the Implementation Opinions put forward by the Provincial Work Safety Bureau on Further Strengthening Work Safety in the Handling of Hazardous Chemicals, the following opinions are hereby presented regarding the standardization of such technical upgrades in chemical enterprises within our province. I. Overall Objectives: Backed by scientific and technological progress and utilizing administrative permits for safe production as a means, the work of upgrading automatic control technologies in chemical enterprises shall be advanced in accordance with the principles of \"safety and reliability, cost-effectiveness, focus on key areas, and phased implementation\". By the end of 2010, chemical enterprises whose production processes involve hazardous techniques or that store highly toxic and flammable/explosive chemicals must complete upgrades to their automatic control systems in order to enhance their safety capabilities. II. Scope of renovation 1. Production facilities: Production facilities involved in hazardous processes such as nitration, chlorination, fluorination, ammoniation, sulfonation, hydrogenation, diazotization, oxidation, peroxidation, cracking, and polymerization. 2. Storage facilities: Tank areas and storage areas for highly toxic, flammable, and explosive chemicals ; Key storage tanks such as liquefied gases and highly toxic liquids that constitute major hazard sources. III. Requirements for renovation: Chemical enterprises whose production units and storage facilities fall within the scope of renovation should, based on factors such as process characteristics, unit scale, storage format, and degree of controllability, install appropriate safety interlocks, alarms for excessive temperatures, pressures, or liquid levels, as well as audio-visual alarms for detecting concentrations of flammable or toxic gases. They should also implement automatic control mechanisms such as automatic pressure relief, emergency shutdown, and emergency interlocked shutdown. In addition, intelligent automated instruments, programmable logic controllers (PLC), distributed control systems (DCS), emergency shutdown systems (ESD), and safety instrumented systems (SIS) can be used to minimize manual operations on site and enhance the level of automatic safety control in the enterprise. 1. New production units or storage facilities constructed within the scope of the renovation must be equipped with automatic control systems. Safe and reliable automatic control instruments and interlock protection systems should be used, in addition to necessary detection and alarm systems for leaks of toxic, harmful, flammable, and explosive gases, as well as fire alarm systems. For investment projects with a scale of 100 million yuan or more, as well as those equipped with production units involving high-risk processes (such as cracking, hydrogenation, polymerization, fluorination, nitration, peroxidation processes, etc.), emergency shutdown systems must be installed in addition to automated control systems. 2. Existing production facilities involving hazardous processes must complete the transformation to automatic control technology within the specified time frame, in order to achieve automatic control of the process flow as well as automatic alarm functions for key parameters such as temperature and pressure. Systems with high risk or under certain conditions must be equipped with distributed control systems and emergency shutdown systems to enable remote operation. Hazardous chemical manufacturing enterprises must complete the renovations before renewing (obtaining) their safety production licenses. 3. The existing storage facilities within the scope of the renovation must complete the upgrade to automatic control technology within the specified time limit. Storage areas for highly toxic and flammable/explosive chemicals must be equipped with alarms for excessive levels of liquid, temperature, and pressure, as well as gas leak detection alarms and fire alarm systems ; Key storage tanks such as liquefied gases and highly toxic liquids, which constitute major hazard sources, must be equipped with emergency shut-off devices. IV. Basic Operating Procedures 1. Confirmation of the modification contents. Enterprises should verify whether their production facilities and storage installations involve any automation control technology upgrades. The safety assessment agency shall include a dedicated section in the assessment report to conduct a specific evaluation of the automatic control systems of the production units and storage facilities, in order to determine whether there are any such units or facilities within the scope of the modifications required. If so, it is necessary to evaluate whether its existing control methods meet the requirements for automatic control, and to draw a clear conclusion as to whether automatic control has been achieved. 2. Formulation of the renovation plan. If it is determined through evaluation that an automatic control technology upgrade is necessary, the enterprise should organize its internal engineering and technical personnel, or invite chemical engineering design firms, entities responsible for implementing the automatic control technology upgrades, safety assessment agencies, and relevant experts to conduct a hazard analysis of the relevant production facilities or storage units. Key control points shall be identified, and the chemical engineering design firm or the entity responsible for the upgrade, in conjunction with the safety assessment agency, shall prepare a plan for the automatic control technology upgrade based on the results of the hazard assessment. After the plan is prepared, the enterprise must organize relevant experts, chemical engineering design firms, units responsible for implementing automatic control upgrades, and safety assessment agencies to evaluate the plan. 3. Implementation of the renovation project. Enterprises should commission entities with the appropriate qualifications for carrying out automatic control technology upgrades, and select safe, reliable, and certified safety instrument products. The entity responsible for implementing the automation control technology upgrades shall carry out the installation and testing of safety instruments in accordance with the approved upgrade plan, as well as the trial operation of the automated control system after such installation and testing; it is also responsible for training the relevant engineering and technical personnel as well as operators within the enterprise. For the commissioning of automatic control systems, enterprises must work together with the units responsible for the technical upgrades related to automatic control to develop comprehensive plans for shutting down and starting up the systems before and after commissioning. It is also necessary to implement all appropriate safety measures to ensure the safety of these shutdown and startup processes. Once the automatic control system is operating properly, the enterprise is responsible for its daily maintenance. For the testing and inspection of safety instruments, those that are required by law must be carried out by qualified organizations; other tasks can be entrusted to entities specialized in automatic control technology upgrades. 4. Acceptance of the renovation project. After the trial operation of the automatic control system is completed, the enterprise should assemble relevant experts, chemical engineering design firms, entities responsible for implementing the automatic control technology upgrades, and safety assessment agencies to conduct an acceptance inspection of the project, and prepare a written report on the results of this inspection. Inform the local safety supervision department in writing after the acceptance is completed. V. Responsibilities of Relevant Entities 1. Chemical enterprises involved in automated control technology upgrades shall earnestly organize and implement such upgrades in accordance with the requirements of these guidelines. Those that fail to complete the automation control technology upgrades within the specified time limit must suspend production for rectification. Enterprises bear the primary responsibility for automatic control renovation work. 2. Safety assessment agencies shall, based on the actual situation of the enterprise, determine in a realistic manner whether the enterprise is involved in automation control technology upgrades. Participate in the hazard analysis and assessment of the production units or storage facilities undergoing modification, identify key control points, prepare implementation plans for the modifications, and take part in the acceptance testing of these modifications. The safety assessment agency is responsible for confirming the contents of the modifications and undertaking the related work. 3. The chemical engineering design firm is responsible for preparing an implementation plan for the automation control upgrades, and such a plan must take into account the actual conditions of the enterprise’s production facilities and storage systems. Participate in the hazard analysis and assessment of the production units or storage facilities undergoing modification, identify key control points, and take part in the acceptance testing of the modification work. The chemical engineering design firm is responsible for designing the implementation plan for the automation control technology upgrade and carrying out the related tasks. 4. The entity responsible for the implementation of the automatic control technology upgrade is in charge of the construction of such upgrade projects. Ensure that safety instruments are installed and tested in accordance with requirements, and that the automatic control systems operate properly; also ensure that the relevant engineering and technical personnel as well as operators in the enterprise have thorough knowledge of these automatic control systems. Participate in conducting hazard analysis and assessment of the production units or storage facilities undergoing renovation, identifying key control points, preparing implementation plans for the renovations, and taking part in the acceptance of these renovation projects. The entity responsible for the implementation of the automatic control technology upgrade is accountable for the quality of the project, the quality of the safety instrumentation systems used, as well as the related tasks undertaken. VI. Requirements for the technological transformation using automatic control techniques 1. All regions shall, in accordance with the requirements of this notice, further identify the list of chemical enterprises within their jurisdictions that are subject to technological transformation using automatic control techniques, develop corresponding work plans, and accelerate the implementation of such transformations. Enterprises involved in the technological upgrading of automatic control systems should be urged to promptly develop upgrade plans, and to adopt appropriate automatic control methods or systems based on actual conditions. 2. All regions should establish a work schedule for implementing automated control technology upgrades in the chemical enterprises within their jurisdictions, and carry out these upgrades in phases. At present, it is necessary to focus on carrying out the automation control technology upgrades for hazardous chemical manufacturing enterprises whose licenses are due for renewal, to ensure that these upgrades are completed before the renewal process. 3. All regions should urge enterprises to ensure proper qualification verification of relevant units and personnel; all chemical engineering design firms, entities responsible for the implementation of automatic control technology upgrades, safety assessment agencies, or related personnel involved in such upgrades must possess the appropriate qualifications as stipulated. The unit responsible for the construction work must hold a qualification level of three or higher for professional contracting in the installation of mechanical and electrical equipment, or for the installation of petrochemical equipment and pipelines, and must also possess a \"Work Safety License\" issued by the construction authorities. 4. All regions should make the implementation of automatic control in new, modified, and expanded construction projects related to production facilities that employ hazardous processes as well as key storage facilities a condition for granting administrative permits for safe production, thereby ensuring strict controls on safety access. For new, modified, and expanded construction projects involving production units and storage facilities within the scope of renovation, corresponding automatic control systems must be designed, installed, and put into use simultaneously. Those that have not undergone safety reviews or safety facility design reviews must develop or design corresponding automatic control systems; otherwise, they will not pass the review ; For those that have already entered trial production, corresponding automated control system upgrades must be carried out before the end of the trial production period; otherwise, the acceptance inspection for safety facilities will not be approved. 5. Chemical manufacturing enterprises that have completed automatic control technology upgrades prior to the issuance of these guidelines shall organize relevant experts to conduct an inspection of the upgrades. For those that do not meet the requirements stipulated in these guidelines, local work safety supervision departments shall urge enterprises to make timely modifications and adjustments. 6. To standardize the technical upgrades related to automatic control, the provincial authority has compiled the \"Suggestions for Technical Upgrades in Automatic Control of Hazardous Processes\" (see attachment), which lists some typical process types along with the recommended automatic control methods for reference by various regions during implementation. May 20, 2009
Attachment: Recommendations for technological upgrades in automatic control of hazardous processes 1. Chlorination process Process overview: A reaction process in which chlorine atoms are introduced using organic and inorganic chlorides such as chlorine, hydrogen chloride, and thionyl chloride. Typical processes: (1) Chlorination reaction with chlorine: for example, the reaction of yellow phosphorus with chlorine to produce phosphorus trichloride, and the reaction of acetylene with chlorine to produce 1,2-dichloroethylene ; (2) Chlorination reaction of hydrogen chloride: For example, the addition reaction of acetylene and hydrogen chloride produces vinyl chloride. It is recommended to install an automatic control system: over-temperature, over-pressure, leakage alarm, and automatic shut-off systems, etc. (Key control parameters: temperature, pressure, flow rate, concentration of toxic and harmful gases, etc.). 2. Pyrolysis process: Process overview: In chemical production, it is the reaction process in which large molecular organic compounds are converted into smaller molecular organic compounds through thermal pyrolysis or catalytic pyrolysis. Typical process: (1) Alkane cracking: Isobutane cracking to produce propylene and methane, or butylene and hydrogen. (2) Olefin cracking: Pentene cracking to produce propylene and ethylene ; Production of cyclohexene via the cracking of butadiene and ethylene ; Butene is cracked to produce butadiene and hydrogen. (3) Naphthenes cracking: Cracking cyclohexene to produce ethylene and butylene ; Naphthalane cracking produces cyclohexene and butylene. (4) Aromatic hydrocarbon cracking: Propylbenzene cracking to produce benzene and propylene, or toluene and ethylene ; Ethylbenzene is cracked to produce styrene and hydrogen. It is recommended to install automatic control systems such as DCS and ESD systems (key control parameters: temperature, pressure, flow rate, concentration of flammable and explosive gases, etc.). 3. Sulfonation process: Process overview: The sulfonation process is a reaction in which sulfonyl groups are introduced into organic compound molecules. It includes methods such as sulfur trioxide sulfonation, azeotropic dehydration sulfonation, chlorosulfonic acid sulfonation, baking sulfonation, and sulfite sulfonation. Typical process: (1) Sulfur trioxide sulfonation method: *** and liquid sulfur trioxide are used to produce *** sulfonic acid ; Toluenesulfonation is used to produce p-sulfonic acid and p-cresol ; p-Nitrotoluenesulfonation is used to produce o-p-nitrotoluenesulfonic acid. (2) Chlorosulfonic acid sulfonation method: Aromatic compounds react with chlorosulfonic acid to produce arylsulfonic acids ; Aromatic compounds react with excess chlorosulfonic acid to form arylsulfonyl chlorides ; Acetanilide and chlorosulfonic acid are used to produce p-acetamidobenzenesulfonyl chloride. It is recommended to install an automatic control system: including alarms for overheating, overpressure, and leaks of toxic or harmful gases, as well as an automatic shutdown system (key control parameters: temperature, pressure, flow rate, concentration of toxic or harmful gases, etc.). 4. Hydrogenation process: Process overview: The reaction process of adding hydrogen atoms to organic compound molecules. Typical process: (1) Hydrogenation of unsaturated alkynes and olefin double bonds: Catalytic hydrogenation of acetylene to produce ethylene and ethane ; Cyclopentadiene is hydrogenated to produce cyclopentene. (2) Aromatic hydrogenation: Hydrogenation of benzene to cyclohexane ; Hydrogenation of styrene to ethylcyclohexane ; Hydrogenation of phenol to cyclohexanol. It is recommended to install automatic control systems such as DCS and ESD systems (key control parameters: temperature, pressure, flow rate, concentration of flammable and explosive gases, etc.). 5. Polymerization Process: Process overview: Polymerization is a reaction in which one or several small molecular compounds are converted into large molecular compounds (also known as polymers, with typical molecular weights ranging from 1×104 to 1×107). The technological process involved in such polymerization reactions is referred to as the polymerization process. There are many types of polymerization processes. Based on the polymerization method, they can be classified into bulk polymerization, suspension polymerization, emulsion polymerization, solution polymerization, etc. Typical process: (1) Bulk polymerization: Production of high-pressure polyethylene from ethylene. (2) Solution polymerization: Synthesis of polyacrylamide using acrylonitrile as a raw material ; Production of polyvinyl acetate from vinyl acetate (VAC) ; Acrylate coatings, adhesives, etc. (3) Emulsion polymerization: Emulsion polymerization of butadiene and styrene to produce SBR. (4) Suspension polymerization: Preparation of polyvinyl chloride by the vinyl chloride suspension method. It is recommended to install automatic control systems such as DCS and ESD systems (key control parameters: temperature, pressure, flow rate, concentration of flammable and explosive gases, etc.). 6. Diazotization process: Process overview: Diazotizing agents are produced by reacting sodium nitrite with inorganic acids such as hydrochloric acid, sulfuric acid, perchloric acid, and fluoroboric acid; these agents then react with primary amines present in aliphatic, aromatic, and heterocyclic compounds to form diazonium compounds. The process involved in the aforementioned reaction is the diazotization process. Typical process: (1) Direct method: Preparation of Acid Orange-II dye from sodium p-aminobenzenesulfonate and 2-naphthol ; Aromatic primary amines react with sodium nitrite to produce aromatic diazonium compounds. (2) Anti-addition: Production of m-phenylenediamine diiodoborate from m-phenylenediamine ; Aniline reacts with sodium nitrite to produce anilino-diazobenzene. (3) Nitrosyl sulfate method: Preparation of monoazo dyes from aniline derivatives ; Blue disperse dyes are prepared using 2-cyano-4-***amine as a starting material. It is recommended to install an emergency control system: over-temperature and over-pressure alarms and automatic shut-off mechanisms, automatic emergency cooling systems (such as the use of ice), automatic emergency discharge systems, etc. (Key control parameters: temperature, pressure, flow rate, etc.). 7. Fluorination Process: Process overview: Fluorination is a reaction in which fluorinating agents such as fluorine, halogen fluorides, fluorides of inert elements, hydrogen fluoride, and potassium fluoride are used to introduce fluorine into organic compound molecules; the process involved in such fluorination reactions is known as the fluorination process. Typical process (direct fluorination): Concentrated sulfuric acid and calcium fluoride (fluorite) are used to produce anhydrous hydrogen fluoride ; Phosphorus pentafluoride is prepared by fluorination of yellow phosphorus. It is recommended to install emergency control systems such as DCS and ESD systems (key control parameters: temperature, pressure, flow rate, concentration of toxic and harmful gases, etc.). 8. Nitration Process: Process overview: The nitration process refers to the reaction in which nitric acid, mixed acids (mixtures of nitric acid and sulfuric acid), or mixtures of nitric acid and anhydrides are used as nitrating agents to introduce nitro groups (-NO2) into organic compound molecules. It usually includes pot nitration, adiabatic nitration, pump nitration, tubular nitration, etc. Typical processes and recommended installation of emergency control systems: (1) Direct nitration with nitric acid: Nitration of glycerin to produce nitroglycerin ; Synthesis of o-nitro-p-cresol from cresol and nitric acid in dichloromethane ; 1-Nitroanthraquinone is prepared by the nitration of anthraquinone. (2) Mixed-acid nitration: Nitration of anthraquinone to prepare 1-nitroanthraquinone ; Nitration of chlorobenzene to produce o-nitrochlorobenzene, p-nitrochlorobenzene, and m-nitrochlorobenzene ; Preparation by nitration of benzene*** ; Acetanilide is nitrated to produce nitroacetanilide and similar compounds. It is recommended to install emergency control systems: DCS, ESD, and other such systems (key control parameters: temperature, pressure, flow rate, etc.). 9. Oxidation process: Process overview: Oxidation is the process of losing electrons in a chemical reaction involving electron transfer, that is, a process in which the oxidation state increases. A process involving oxidation reactions is an oxidation process. Common oxidizing agents include: air, oxygen, hydrogen peroxide, potassium chlorate, potassium permanganate, nitrates, etc. Typical process: (1) Catalytic oxidation reaction involving air: Ethylene can be converted into ethanol, acetaldehyde, ethyl alcohol, and acetic acid through oxidation ; Oxidation of toluene to benzoic acid ; P-xylene is oxidized to produce terephthalic acid, etc. (2) Chemical oxidation: Oxidation of p-chlorotoluene to produce p-chlorobenzaldehyde ; Toluene is oxidized to produce benzaldehyde and others. It is recommended to install an automatic control system: over-temperature, over-pressure, leakage alarms, and automatic shut-off systems, etc. (Key control parameters: temperature, pressure, flow rate, etc.). 10. Peroxidation process: Process overview: The reaction in which a peroxide group (-O-O-) is introduced into organic compound molecules is called a peroxidation reaction. Processes that involve peroxides such as hydrogen peroxide and organic peroxides are referred to as peroxidation processes. Typical process: (1) Hydrogen peroxide as an oxidant: Acetic acid reacts with hydrogen peroxide in the presence of sulfuric acid to produce an aqueous solution of peracetic acid ; The reaction of anhydrides with hydrogen peroxide can directly produce peracid and similar compounds. (2) Organic peroxides as oxidants: Epoxidation of propylene to propylene oxide ; Isopropylbenzene is oxidized by air to produce isopropylbenzene peroxide and others. It is recommended to install automatic control systems such as DCS and ESD systems (key control parameters: temperature, pressure, flow rate, etc.). 11. Ammoniation process: Process overview: Ammonolysis and amination are often referred to as aminoation. Ammonolysis refers to the double displacement reaction between ammonia and inorganic or organic substances, while amination is the reaction that introduces amino groups (NH2-) or ammonium groups (R2N-) into molecules. The aforementioned reaction process is the ammoniation process. Typical process (ammonolysis process): O-nitrochlorobenzene reacts with ammonia water to produce o-***amine ; Methanol is used, under the action of a catalyst and ammonia, to produce methamine and other substances. It is recommended to install an automatic control system: over-temperature, over-pressure, leakage alarm, and automatic shut-off systems, etc. (Key control parameters: temperature, pressure, flow rate, concentration of flammable and explosive gases, etc.). 12. High-risk storage tanks: Scope of renovation: Areas where highly toxic, flammable, and explosive chemicals are stored ; Key storage tanks such as liquefied gases and highly toxic liquids that constitute major hazard sources. It is recommended to install an emergency control system: alarms for excessive liquid level, temperature, and pressure, gas leak detection alarms, and a fire alarm system ; Key storage tanks such as liquefied gases and highly toxic liquids, which constitute major hazard sources, must be equipped with emergency shutdown systems (key control parameters: temperature, pressure, concentration of toxic, harmful, flammable, and explosive gases, etc.).
I’m really confused; it should be a private company. Do legitimate companies use wooden barrels for chemical processing? Unless it’s a snap reaction. If the volume is small, automation may not be necessary. Especially when a company currently has a low level of automation, the upfront costs for automating a certain piece of equipment – such as installing piping racks and purchasing electrical and control devices – are relatively high. Look at the investment/return!
I’ve heard of this kind of reaction from the original poster for the first time. If that’s indeed the case, operating at open pressure and low temperature involves relatively low risks; however, if something goes wrong and the barrel breaks, it could lead to serious accidents. Based on the above principles, it seems that such a container is necessary.
Automation is a trend that raises the barriers in the chemical industry
In my opinion, if the reaction takes place in an open wooden barrel, then according to regulatory requirements, a self-control device (to regulate the liquid level) should be installed to prevent overflow; As well as automatic interlocking devices for emergency response in the event of an accident, etc. And isn’t it a bit odd to use wooden barrels as reaction vessels?……
The technique used by the poster (let’s call it a technique for now) is quite distinctive; such a technique should present a low risk of explosion (although it can still cause an explosion if a large amount is used), but it is likely to pose significant environmental hazards. And the operators have a tough time; there are primary amines of aromatic or fatty types, nitrites, nitrous acid that is formed, and nitrogen oxides that are generated, all in an open system where stirring is done manually, probably with sticks. . . I hope it’s just a joke post. . .
A necessary temperature detection and alarm device is still essential