19results about "Nitrous acid preparation ester preparation" patented technology

Disclosed is a process for the synthesis of mono- and bis-nitrosylated propanediols, as well as compositions and pharmaceutical formulations that includes the compounds. The process proceeds by reacting a corresponding propanediol that is not nitrosylated with a source of nitrite, optionally in the presence of a suitable acid. When the source of nitrite is an organic nitrite, reacting step is performed in a suitable organic solvent, and when the source of nitrite is an inorganic nitrite, the reacting step is performed in a bi-phasic solvent mixture comprising an aqueous phase and a non-aqueous phase. Also disclosed are methods of treating a condition wherein administration of nitric oxide (NO) has a beneficial effect by administering said compounds, compositions or formulations.

The invention discloses a method for preparing methyl nitrite through nitric acid reduction, belongs to the technical field of methyl nitrite preparation, and aims to solve the technical problem that the nitric acid conversion rate and the reaction selectivity of the methyl nitrite prepared through nitric acid reduction in the prior art need to be further improved. The preparation method specifically comprises the following steps: roasting and activating a mixed catalyst, and uniformly stirring to obtain an activated catalyst. Through preparation of the active catalyst, construction of a composite network, optimization of a pore structure and metal dispersion through hydrothermal treatment and calcination in the preparation process, and rapid generation of NO < + > at a copper site in the reaction process, the preparation process is simple, and the preparation process is convenient. The catalyst diffuses to tin sites and performs nucleophilic substitution with methanol to generate methyl nitrite, proton feedback drives NO < + > to be continuously generated, efficient mass transfer is ensured by utilizing regular pore channels, the conversion rate of nitric acid and the selectivity of methyl nitrite are remarkably improved through the synergistic effect of Cu-Sn, side reactions are reduced, and the catalyst is suitable for industrial production.

The utility model relates to the field of a dimethyl oxalate synthesis process, in particular to a nitric acid feeding line and dimethyl oxalate production equipment, an original nitric acid liquid inlet subline is cancelled, and a nitric acid boundary valve is arranged at the output end of a nitric acid feeding system to control the flow of nitric acid entering a specific area or system, so that the nitric acid is ensured to flow in a specified range; it is ensured that nitric acid can stably and continuously enter the next link through a nitric acid feeding valve; through the arrangement of the nitric acid drainage regulating valve and the check valve behind the nitric acid feeding valve, after nitric acid supplementing is stopped, the nitric acid in the pipeline is released through the nitric acid drainage regulating valve, nitric acid accumulated liquid stored in the pipeline is avoided, and therefore the situation that the nitric acid flows backwards and reacts with liquid stored in the pipeline is doubly avoided; and the safety of the pipeline is further improved. The problem that the accident risk is high due to the fact that nitric acid feed of an existing nitric acid reduction tower accumulates in a pipeline and reacts with alcohol-containing liquid of a methyl nitrite regeneration tower reversely into the nitric acid pipeline is solved.

The invention discloses a catalytic synthesis method of methyl nitrite, belongs to the technical field of methyl nitrite synthesis, and is used for solving the technical problem that the selectivity of catalytic synthesis of methyl nitrite in the prior art needs to be further improved. The catalytic synthesis method specifically comprises the following steps: adding lanthanum nitrate, copper nitrate, palladium chloride and deionized water into a beaker; the preparation method comprises the following steps: adding amino graphene and aluminum silica gel into a reaction kettle, stirring at room temperature for 10-20 minutes, adding ethylene glycol, continuously stirring for 15-30 minutes, adding a composite carrier into a system, adjusting the pH value to 3-4 by using saturated dilute nitric acid, heating to 50 DEG C, reacting for 12-15 hours, and performing post-treatment to obtain the modified catalyst. The reaction conversion rate, selectivity and catalyst stability are improved.

The present invention provides a method for continuously and adiabatically synthesizing isopropyl nitrite. Under normal temperature and pressure, using sodium nitrite, isopropyl alcohol, and nitric acid as raw materials, and water as a solvent, by controlling the feed volume flow rates of the three raw materials, they are preheated or precooled to the reaction temperature in a heat exchanger, mixed in a micro-sieve pore reactor, and then reacted in an adiabatic reaction tube to finally obtain isopropyl nitrite. The synthesis process of the present invention is simple, the reaction conditions are mild, the reaction time is very short, the product yield and purity are high, the yield reaches more than 97%, the purity reaches more than 98.5%, the production cost is low, the reaction process is safe and reliable, and it is environmentally friendly, solving the technical problems of difficult reaction control, large water consumption, and high harmfulness existing in the existing preparation methods of isopropyl nitrite, and belongs to the technical field of organic synthesis.

The invention discloses a method for preparing methyl nitrite through a reaction of NO and methanol, belongs to the technical field of methyl nitrite, and aims to solve the technical problems that in the process of preparing methyl nitrite through a reaction of NO and methanol in the prior art, the conversion rate, the selectivity and the purity of converting NO into methyl nitrite need to be further improved. The method specifically comprises the following steps: filling a catalyst in a catalytic section of a reaction tower protected by nitrogen, raising the temperature of the catalytic section of the reaction tower to 50-60 DEG C, and raising the pressure of the reaction tower to 0.1-0.2 MPa; according to the method, reaction parameters in the process of preparing the methyl nitrite through the reaction of the NO and the methanol are optimized, so that the conversion rate and the selectivity of converting the NO into the methyl nitrite are effectively improved, the by-product process is reduced, the content of water, nitric acid and other impurities in the prepared methyl nitrite is extremely low, and the method is suitable for industrial production. The catalyst can be directly suitable for reacting with CO to prepare dimethyl carbonate.

The present invention relates to a novel process for synthesizing mono- and bis-nitrosylated propanediols, as well as novel compositions and pharmaceutical formulations containing these compounds. The process proceeds by reacting the corresponding unnitrosylated propanediol with a source of nitrite, optionally in the presence of a suitable acid. When the source of nitrite is an organic nitrite, the reaction step is carried out in a suitable organic solvent; when the source of nitrite is an inorganic nitrite, the reaction step is carried out in a biphasic solvent mixture containing an aqueous phase and a non-aqueous phase. The present invention also relates to methods for treating conditions in which administration of nitric oxide (NO) has a beneficial effect by administering such compounds, compositions, or formulations.

The application relates to the technical field of nitrite synthesis, and discloses a synthesis method and a synthesis device of alkyl nitrite. The synthesis method comprises the following steps: firstly, mixing gaseous nitric oxide and gaseous oxygen to obtain a mixture through a first reaction; and then, mixing the mixture with alkyl alcohol to obtain alkyl nitrite through a second reaction. The synthesis method greatly shortens the reaction time, increases the yield of alkyl nitrite, does not have a complicated post-treatment process and a large amount of by-product nitric acid, and is beneficial to cost saving and time saving.

The invention relates to the field of gas-liquid reaction, in particular to a horizontal reactor and a reaction method using the horizontal reactor. The horizontal reactor is provided with a liquid-phase material inlet and a liquid-phase material outlet along the axial direction; n groups of inlet partition plates and outlet partition plates are axially arranged on the horizontal reactor to divide the horizontal reactor into n + 1 stages of reaction units, and n is an integer greater than or equal to 1; each of the n + 1 stages of reaction units is independently provided with a gas-phase material inlet, a gas distributor and a gas-phase material outlet, and a gas-phase material enters the reaction units through the gas distributors via the gas-phase material inlets. According to the horizontal reactor provided by the invention, the conversion efficiency of materials is effectively improved, the reaction time is shortened, no running part is arranged in the reactor, and the reactor is easy to seal and operate.

The invention discloses a method and a device for efficiently producing methyl nitrite. The method comprises the following steps: carrying out a reaction for generating methyl nitrite in a reaction chamber A to obtain a liquid-phase material, and transferring nitric acid out of the liquid-phase material in the reaction chamber A through an acid transfer concentration device; wherein the liquid-phase material after the nitric acid is transferred serves as a reaction raw material and is reused in the reaction chamber A; transferring the transferred nitric acid into a reaction chamber B; when the mass concentration of the nitric acid in the reaction chamber B is larger than or equal to a first set value, the reaction of converting the nitric acid into methyl nitrite is carried out in the reaction chamber B; when the mass concentration of the nitric acid in the reaction chamber B is less than or equal to a second set value, stopping the reaction for generating the methyl nitrite; the first set value is greater than the second set value. According to the device and the method, oxidative esterification and nitric acid conversion reaction can be simultaneously carried out, methyl nitrite is efficiently produced, the total space-time yield of the product is improved, and the process energy consumption and cost are reduced.

A synthesis method for sodium azide, comprising: using an aromatic alcohol as a raw material to prepare an alkyl nitrite of the aromatic alcohol; under alkaline conditions, reacting the alkyl nitrite with a hydrazine hydrate in a reduction reaction, to prepare sodium azide, the aromatic alcohol comprising one or more compounds having the structural formula represented as: (I), Ar being selected from any one of the following: substituted or unsubstituted C6-C20 aryl groups, and substituted or unsubstituted C3-C10 heteroaryl groups, R being selected from (II) and n being an integer of 1-3; in (III), R1 and R2 are the same or different, and are independently selected from any one of H and C1-C3 alkyl groups; when Ar is selected from substituted C6-C20 aryl groups or substituted C3-C10 heteroaryl groups, substituents of the substituted groups are selected from C1-C9 alkyl groups, and * represents a connection site.

The invention relates to the field of gas-liquid reaction, and discloses a circulation reaction device and a reaction method using the circulation reaction device. The circulation device comprises at least one stage of circulation reactor, the circulation reactor comprises a cylinder body and a guide cylinder arranged in the cylinder body, and an annular space is formed between the cylinder body and the guide cylinder; the loop reactor is provided with a liquid-phase material inlet, a gas-phase material inlet and a gas distributor, and a gas-phase material enters the guide cylinder through the gas distributor via the gas-phase material inlet. Gas-phase materials are sprayed into the guide cylinder to form air lift, liquid is pushed to circularly flow along the guide cylinder, meanwhile, liquid-phase series feeding and gas-phase parallel feeding of all stages of reactors are achieved, it is effectively guaranteed that the materials in all stages of reactors react under the optimal process condition, the gas-liquid contact effect and the mass transfer effect are improved, and the material conversion efficiency is remarkably improved.

The invention belongs to the technical field of process tail gas treatment, and particularly relates to a natural gas-to-ethylene glycol process tail gas treatment method which comprises the following steps: 1) enabling purge gas at the top of an esterification tower to enter an MN absorption area at the top of the esterification tower, and spraying the purge gas with methanol at 30-40 DEG C to obtain coarsely treated purge gas; and 2) feeding the roughly treated purge gas to an MN recovery tower, simultaneously conveying factory air or oxygen to the MN recovery tower, spraying methanol at 15-20 DEG C to the upper part of the MN recovery tower, maintaining the pressure in the MN recovery tower to be 0.2-0.25 MPa, and discharging the treated tail gas from the top of the MN recovery tower. The process tail gas is subjected to two-stage treatment, the MN content of the tail gas discharged from the top of the MN recovery tower is lower than 0.02%, and meanwhile, the CO2 content of the tail gas can reach 3.7%, so that efficient recovery and utilization of the MN effective gas can be guaranteed, the emission of CO2 can be increased, the energy consumption of the device can be reduced, and the efficiency of the device can be improved.

A polynitroso compound, the polynitroso compound comprising a monocyclic core or a polycyclic core to which two or more terminal nitroso groups are attached, such as formula (A) to formula (D), especially formula (VII). A method for preparing the polynitroso compound of the present invention. An energy storage device, the energy storage device having a cathode comprising the polynitroso compound of the present invention. There is also provided an electrode material for an energy storage device, the electrode material comprising a polynitroso compound having a monocyclic core containing at least one terminal nitroso group, such as formula (A) to formula (D), especially formula (VII).

The invention discloses a methyl nitrite regeneration tower based on a gas circulation supply mechanism, relates to the technical field of methyl nitrite regeneration, and aims to solve the problems that an emergency supply mechanism is lacked, the reaction in the tower is difficult to stably control and the nitric acid conversion rate is low due to insufficient gas-liquid contact when gas and a pump are stopped. On one hand, a gas circulation mechanism is matched with a gas-liquid countercurrent horizontal pushing composite effect, stable gas-liquid mixing in the methyl nitrite regeneration process is achieved, heat is taken away through circulation gas, meanwhile, heat is absorbed through spraying gasification of a methanol solution, and the temperature is cooperatively controlled; rapid methanol solution compensation is carried out in cooperation with spraying immediately, and dangerous accidents caused by the fact that the methanol concentration exceeds the standard are prevented; and on the other hand, through the gas-liquid mass transfer effect of variable-pitch and rotatable inlet circulating synthesis gas, turbulent flow changes of the transmission rate and the transmission direction of the synthesis gas can be carried out during secondary gas supply, and finally, the regeneration efficiency of methyl nitrite is improved.

This utility model belongs to the technical field of syngas-to-ethylene glycol process technology, specifically relating to an apparatus for preparing methyl nitrite based on fuming nitric acid, including a booster compressor and a NO... x The generator / absorption tower and nitric acid reduction reaction tower, booster compressor and NO x The bottom gas inlet of the generator / absorber is connected to NO. x The generator / absorber is connected to the nitric acid feed pipe and the demineralized water feed pipe. The top liquid inlet of the nitric acid reduction reaction tower is connected to the bottom liquid pipeline of the esterification tower and the NO... x The bottom liquid phase outlet of the generator / absorption tower is connected, and the bottom gas phase inlet of the nitric acid reduction reaction tower is connected to the NO. x The top gaseous outlet of the generator / absorber is connected. This invention uses fuming nitric acid as raw material to react and obtain NO and nitric acid, which are then reacted with the methyl ester-containing bottom liquid of the esterification tower to generate methyl nitrite, which is then supplied to the esterification tower. This achieves the replenishment of methyl nitrite, simplifies the nitrogen replenishment operation of the syngas to ethylene glycol production system, reduces operational risks, and lowers costs.

The invention discloses a method for continuously and adiabatically synthesizing isopropyl nitrite. The method comprises the following steps: S1, pretreating raw materials; s2, pre-cooling the pretreated raw materials to a reaction temperature; s3, introducing into a micro-channel reactor to form a material flow; s4, nitric acid is injected in a distributed multi-point mode; s5, conveying the mixed material in the reactor to an adiabatic reactor, raising the temperature to 50-80 DEG C by utilizing reaction heat release, and maintaining the pressure at 0.3-0.6 MPa; and step S6, separating the product through a gas-liquid separator, and carrying out gas phase condensation to obtain isopropyl nitrite with the purity of greater than or equal to 98%. Through the design of the microreactor and the control of adiabatic conditions, the reaction time is shortened, and the production efficiency is improved. By optimizing the temperature and the raw material ratio, the yield is increased to 98.1%, and the raw material utilization rate is increased; a continuous flow reaction system avoids the NOx gas accumulation risk of a traditional kettle type process, reaction heat is naturally dissipated through a heat insulation design, and the hidden danger of explosion is eliminated.

The present invention relates to a novel method of synthesizing mononitrosylated and dinitrosylated propanediols and novel compositions and pharmaceutical formulations comprising said compounds. The method is carried out by reacting the corresponding non-nitrosylated propanediol with a source of nitrite, optionally in the presence of a suitable acid. Therein, when the source of nitrite is an organic nitrite, the reaction step is performed in a suitable organic solvent and when the source of nitrite is an inorganic nitrite, the reaction step is performed in a biphasic solvent mixture comprising an aqueous phase and a non-aqueous phase. The present invention further relates to methods of treating conditions in which the administration of nitric oxide (NO) has a beneficial effect, by administering said compounds, compositions or formulations.

Described is a process for the synthesis of mono- and bis-nitrosylated propanediols, as well as compositions and pharmaceutical formulations that includes the compounds. The process proceeds by reacting a corresponding propanediol that is not nitrosylated with a source of nitrite, optionally in the presence of a suitable acid. When the source of nitrite is an organic nitrite, reacting step is performed in a suitable organic solvent, and when the source of nitrite is an inorganic nitrite, the reacting step is performed in a bi-phasic solvent mixture comprising an aqueous phase and a non-aqueous phase. Also disclosed are methods of treating a condition wherein administration of nitric oxide (NO) has a beneficial effect by administering said compounds, compositions or formulations.