38results about "Nitric acid ester preparation" patented technology

The invention discloses application of polyol nitrate in frostbite resistance, and belongs to the technical field of skin protection articles. The polyol nitrate is used as an active component of the ointment, and by slowly releasing nitric oxide and activating vascular endothelial nitric oxide synthase, spasm capillaries in the early stage of frostbite are effectively relaxed, platelet aggregation and thrombosis are inhibited, so that the pathological cascade reaction of frostbite is blocked, and the prevention and treatment effects on frostbite are remarkably improved. Compared with the prior art, the polyol nitrate and the ointment are scientific and reasonable in preparation method and safe and convenient to use, and a brand-new and effective solution is provided for prevention and treatment of skin frostbite in a cold environment.

The invention relates to a method for drying and / or cleaning, preferably drying and cleaning aliphatic or cycloaliphatic nitrate esters (nitrate esters), in particular for removing water and volatile and / or volatilizable impurities, in particular generated during the production and / or washing of nitrate esters, the invention also relates to a corresponding use and to a corresponding device and system for carrying out the method.

The present invention relates to a process for the preparation of α-methyl-[4-(nitro)-2-(trifluoromethyl)]-benzyl nitrate and to the α-methyl-[4-(nitro)-2-(trifluoromethyl)]-benzyl nitrate.

The invention discloses a method for preparing 3-hydroxypropyl nitrate by continuous flow, the 3-hydroxypropyl nitrate is continuously prepared by a three-step method of monoacetylation, nitration and hydrolysis, and the prepared compound can be confirmed by a 1H NMR (nuclear magnetic resonance) characterization method. Meanwhile, through a two-step continuous flow reaction technology and a two-step online continuous separation technology which are connected in series, continuous production is realized, and key reaction parameters such as material mixing, heating and retention time can be accurately controlled, so that the product quality is improved, impurities are controlled, the chemical reaction is allowed to react in a higher temperature range without temperature runaway, and the product quality is improved. The reaction speed can be increased in reaction thermodynamics, the production efficiency is improved, heat accumulation of kettle type reaction is avoided, and the reaction is safer; the post-treatment process of the flow chemistry is always online, so that the reaction is cleaner, automatic and online sample collection is convenient to realize, reaction parameters are convenient to change, optimal reaction conditions are convenient to find, and the process exploration and substrate screening efficiency is greatly improved.

The invention relates to the technical field of chemical engineering, in particular to a preparation method of high-yield isooctyl nitrate. The preparation method comprises the following steps: S1, preparing raw materials; s2, catalytic esterification; s3, separating and washing; according to the method, the additive A coating with phosphotungstic acid loaded ionic liquid is formed on the inner wall of the reactor, proton transfer and selective catalysis in the esterification process are enhanced, the outer wall of equipment is sprayed with the additive B coating with biological fiber compounded phytic acid, and the heat transfer stability and heat loss control of a reaction system are improved; the waste acid water is treated by combining a dilute sulfuric acid gradient concentration-steam stripping coupling system, a continuous production system with high yield and recyclable waste acid is realized, and the production efficiency and product purity of the isooctyl nitrate are effectively improved from the aspects of catalysis principle and process enhancement.

The utility model belongs to the technical field of isooctyl nitrate production equipment, and discloses an isooctyl nitrate crude product alkali washing device which comprises a fiber membrane contactor and a separation tank which are communicated, the top of the fiber membrane contactor is provided with a first liquid inlet pipe used for leading in an isooctyl nitrate crude product and a second liquid inlet pipe used for leading in alkali liquor, and the first liquid inlet pipe and the second liquid inlet pipe are communicated with each other. The first liquid inlet pipe penetrates along the top of the fiber membrane contactor, a buffer mechanism is arranged below the first liquid inlet pipe, the buffer mechanism comprises a splitter plate and a buffer cavity with an opening in the top, a pipe opening of the first liquid inlet pipe is located in the buffer cavity, the buffer cavity is formed in the center of the top of the splitter plate, and through holes are evenly distributed in the splitter plate. According to the utility model, the buffer cavity is matched with the splitter plate to buffer the crude isooctyl nitrate introduced into the fibrous membrane contactor, so that the generation of foam is reduced, and the crude isooctyl nitrate is ensured to be fully deacidified.

The present invention provided a process for manufacture of amantadine nitrate derivatives, and the process comprises using adamantane as the raw material to prepare amantadine nitrate derivatives via the following steps: (1) synthesis of adamantanol; (2) carboxylation of adamantanol; (3) acetylation of adamantanoic acid; (4) reduction; (5) hydrolysis of amido adamantanol and Boc protection of amino group; (6) crystallization of Boc protected amantadinol; (7) nitrate esterification of Boc protected amantadinol; (8) refining of the product of nitrate esterification; (9) Boc deprotection and salt formation; and (10) refining of amantadine nitrate hydrochloride. The amantadine nitrate derivatives have the struction of: wherein, R1 and R2 are each independently hydrogen, straight-chain or branched-chain alkyl, or substituted or unsubstituted aryl or heteroaryl. The process of this invention is efficient, cost effective, environmentally friendly, safe, reliable, and suitable for industrial production.

The utility model relates to the technical field of isooctyl nitrate production, in particular to a dehydration device for isooctyl nitrate production, which comprises a rectangular shell, a placing plate and a stirrer arranged in the shell, a dehydration cylinder arranged on the placing plate, and lifting mechanisms arranged on two sides of the inner wall of the shell, the placing plate is horizontally and slidably arranged in the shell, the stirrer is vertically and slidably arranged in the shell, and the lifting mechanism is in transmission connection with the stirrer to drive the stirrer to vertically move; by arranging the lifting mechanism and the stirrer, the stirrer can vertically move and extend into the dehydration barrel for stirring, it is ensured that isooctyl nitrate and anhydrous sodium sulfate are fully mixed, the stirring efficiency is improved, and the dehydration effect is improved; in the stirring process of the stirrer, the baffle covers the upper part of the dehydration barrel, so that liquid is prevented from splashing in the stirring process, experimenters are prevented from being harmed, and the safety of experimental operation is improved; through the linkage design of the lifting mechanism and the clamping mechanism, automatic clamping of the dewatering cylinder and automatic lifting of the stirrer are achieved.

The invention belongs to the technical field of stabilization of nitrate ester compounds, and particularly relates to application of poly (p-phenylenediamine) as a stabilizer for the nitrate ester compounds, and the addition amount of the poly (p-phenylenediamine) is 2.9%-3.1% on the basis of the total weight of the nitrate ester compounds. The preparation method of the poly (p-phenylenediamine) comprises the following steps: taking ammonium persulfate as an oxidizing agent, taking p-phenylenediamine as a monomer, adopting a spiral gas-solid two-phase flow technology, and enabling raw material solid particles to mutually rub and collide to initiate an oxidative polymerization reaction, so as to prepare the poly (p-phenylenediamine). The poly (p-phenylenediamine) has the characteristics of low price, easiness in synthesis, no toxicity, excellent nitrogen oxide absorption capacity and the like, has good compatibility with nitrate ester compounds, can effectively reduce the autocatalysis phenomenon and improve the long-term stability of the nitrate ester compounds, can avoid the toxicity problem of the traditional amine stabilizer when being used as the stabilizer, and has the advantages of low cost, low cost and the like. The environment and human health are facilitated.

The invention provides a preparation method of a plasticizer based on ionic liquid, and belongs to the technical field of solid propellants. The method comprises the following steps: reacting an alkaline compound with sultone to generate sulfonic acid inner salt, then mixing the sulfonic acid inner salt with nitric acid, and sequentially carrying out reflux condensation and rotary evaporation to obtain the ionic liquid; acetic anhydride and ionic liquid are mixed, then trimethylolethane is added for a reaction, and the plasticizer is obtained. According to the preparation method disclosed by the invention, the ionic liquid is used for replacing the traditional mixed acid, so that the recycling of the reaction is realized, and the generation of three wastes is obviously reduced. In addition, the method can effectively reduce the preparation cost.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of isooctyl nitrate. According to the method, cyclohexane is used as a solvent, urea is used as a stabilizer, composite aerogel is used as a catalyst, and isooctyl nitrate is generated from isooctyl alcohol under the nitration effect of concentrated nitric acid. According to the method, use of sulfuric acid can be avoided, the prepared isooctyl nitrate is high in yield and purity, the whole preparation process is safe and environmentally friendly, and safe and efficient preparation of the isooctyl nitrate can be achieved.

The invention discloses a catalyst for synthesizing nitrous acid ester and a preparation method thereof. The catalyst is composed of the following components: a main active component loaded on a carrier, wherein the main active component is noble metal, and the loading amount is 0.5-5wt% of the mass of the carrier; the carrier is a modified mesoporous molecular sieve, and the loading capacity is 40-60% of the mass of the carrier; the cocatalyst is a rare earth metal oxide, and the loading capacity is 5-15% of the mass of the carrier; the acid catalyst is p-toluenesulfonic acid, and the loading capacity is 0.3%-1.5% of the mass of the carrier. The invention relates to a preparation method and application of a catalyst for synthesizing nitrite, and the catalyst has the beneficial effects that the catalyst is a heterogeneous catalyst which is high in catalytic activity, good in stability and reusable, in an esterification reaction of alcohol and nitrite, the activity of the catalyst is improved by more than 30%, and the reaction time is shortened to 2-4 hours; after the catalyst is recycled for 5 times, the catalytic activity is still kept above 90%; the product selectivity reaches 98% or above, and no complex purification step is needed.

A process for drying and / or purifying, preferably drying and purifying, aliphatic or cycloaliphatic nitrate esters (nitric acid esters), in particular for removing water and volatile impurities, especially those arising during the production and / or washing of the nitrate esters, wherein the process comprises the following process steps: (a) first, the crude nitrate esters obtained from a production process are subjected to washing with a washing medium, followed by separation of the washing medium; (b) subsequently, the washed crude nitrate esters obtained in process step (a) are subjected to drying and / or purification, preferably drying and purification, by contact, in particular by flowing, with an inert gas, in particular such thatthat water present in the washed crude nitrate esters is removed and, at the same time and / or in the same way, volatile impurities arising in particular during the production and / or washing of the nitrate esters are removed.

The present invention relates to a process for the preparation of 6-(nitrooxy)-hexanoic acid (1S,2E)-3-[(1R,2R,3S,5R)-2-[(2Z)-7-(ethylamino)-7-oxo-2-hepten-1-yl]-3,5-dihydroxycyclopentyl]-1-(2-phenylethyl)-2-propen-1-yl ester of formula (I). According to the present invention, the compound (I) can be efficiently prepared in high purity by coupling bimatoprost in boronate protected form with 6-(nitrooxy)hexanoyl chloride and removing the boronate protecting group. The present invention also relates to a process for the preparation of 6-(nitrooxy)hexanoic acid having a HPLC purity equal to or greater than 99% and containing 6-{[6-(nitrooxy)hexanoyl]oxy}hexanoic acid (compound (IXa)) in an amount equal to or lower than 0.2%.

The invention discloses pentaerythritol tetranitrate, a preparation method and application thereof and a solid superacid catalyst recovery method, and the preparation method comprises the following steps: grinding a solid superacid catalyst to obtain catalyst particles with the average particle size of 20 nm <-1 > [mu] m; the catalyst particles, pentaerythritol and fuming nitric acid are mixed according to the mass ratio of (0.005-0.1): 1: (2-4), and reaction liquid slurry is formed; introducing the reaction slurry into an ultrasonic-assisted microchannel reactor, and carrying out continuous two-stage temperature-controlled nitration reaction under the action of ultrasonic waves with the frequency of 20-150KHz; the nitration reaction at least comprises two temperature stages; and collecting a reaction product solution generated from the ultrasonic-assisted microchannel reactor to obtain the pentaerythritol tetranitrate. The method is suitable for large-scale application in the field of energetic material preparation.

The application provides a method for treating TPU solid waste by using molten sodium salt and preparing nitrate, and belongs to the field of solid waste treatment. The method solves the problems of high risk and high cost in traditional molten salt method for recycling TPU. The method comprises the following steps: S1, drying Na2CO3-NaOH at a certain drying temperature for a certain time to remove excess water, mixing the dried Na2CO3 and NaOH at a certain proportion to form a Na2CO3-NaOH system, and placing the Na2CO3-NaOH system in a molten salt reaction kettle; S2, heating the molten salt reaction kettle to a certain temperature and keeping the temperature for a certain time until the Na2CO3-NaOH system is completely melted; S3, putting TPU solid waste in a certain proportion with the Na2CO3-NaOH system into the molten salt reaction kettle, and reacting for a certain time to form waste salt; S4, collecting liquid products in the tail gas gas phase of the molten salt reaction kettle. The waste salt is washed with water and filtered to obtain a liquid sample, the liquid product and the liquid sample are characterized in terms of composition and content, and the content of nitrate in the liquid product and the liquid sample is determined. The method is mainly used for treating TPU solid waste.

The invention provides bicyclo [1.1. 1] pentane-1, 3-dimethylene dinitrate as well as a preparation method and application thereof, and belongs to the technical field of functional materials. The invention aims to solve the technical problems of insufficient energy density, poor thermal stability or complex synthesis process of plasticizers. The preparation method comprises the following steps: (1) carrying out esterification reaction on a compound 1 to obtain a compound 2; (2) mixing the compound 2, a reducing agent and a solvent for reduction reaction to obtain a compound 3; and (3) nitrating the compound 3 to obtain a product compound 4. According to the bicyclo [1.1. 1] pentane-1, 3-dimethylene dinitrate, high-tension propeller alkane is used as a framework, meanwhile, a nitrate ester functional group is introduced, and the bicyclo [1.1. 1] pentane-1, 3-dimethylene dinitrate has high energy density and good thermal stability and can be used as an energetic plasticizer in a solid propellant. Compared with a traditional plasticizer DEHA, the mechanical property and the thermal stability of a sample strip cured in an HTPB-TDI system are improved.

The application belongs to the technical field of organic synthesis, and particularly relates to a preparation method of isooctyl nitrate. The method uses cyclohexane as a solvent, uses urea as a stabilizer, and uses a composite aerogel as a catalyst, so that isooctanol is nitrified by concentrated nitric acid to generate isooctyl nitrate. The method can avoid the use of sulfuric acid, and the prepared isooctyl nitrate has high yield and high purity, the whole preparation process is safe and environmentally friendly, and safe and efficient preparation of isooctyl nitrate can be realized.

The invention discloses a system for flexibly preparing nitrate ester. The system comprises a Meilan acid storage tank, a fuming sulfuric acid storage tank, a first acid mixing ejector, a second acid mixing ejector, a first acid cooler, a second acid cooler, a polyhydric alcohol storage tank, a spraying nitrator, a coil pipe cooler, a kettle type continuous overflow nitrator, a centrifugal separator, a first dynamic washing separator and a second dynamic washing separator. The device comprises a first dynamic washing separator, a second dynamic washing separator, a third dynamic washing separator, a jet conveyor, a jet conveying water tank, a nitrate finished product temporary storage tank, a wastewater curved channel device, a nitrate-containing waste acid temporary storage tank, a flow meter, a gear pump, a three-way valve A, a three-way valve B, a three-way valve C and a three-way valve D, according to the system for preparing the nitrate ester, the nitrate ester can be prepared by selecting a spraying nitration process or a kettle type continuous overflow nitration process according to the characteristics of the nitrate ester.

The invention relates to a safe and efficient process for the for the acylation of an α,ω-alkanediol, which can be used in the manufacture of ω-nitrooxy-C3-10alkane-1-ols. The process is safer to operators and allows to obtain advantageous yields on industrial scale.

The application provides a hydroxyl-substituted treprostinil derivative, a synthesis method and application thereof, and belongs to the technical field of drugs.The compound is a coupling compound containing treprostinil and a nitric oxide donor, and is shown as follows.The hydroxyl-substituted treprostinil derivative is a combination drug of treprostinil and a NO donor, solves defects of weak curative effect of treprostinil, inconvenience of NO administration, and uncontrollable dosage, and improves the effectiveness of the drug and the compliance of patients through synergistic effect of the two, and the drug effectiveness control is also improved.

The invention relates to the technical field of chemical waste acid treatment, in particular to a waste sulfuric acid purification treatment process in an isooctyl nitrate production process, which comprises the following steps: S1, carrying out primary treatment on a byproduct waste sulfuric acid in isooctyl nitrate production to obtain primary impurity-removed waste acid; s2, carrying out secondary treatment on the waste acid subjected to primary impurity removal by using a composite treatment agent to obtain pretreated waste acid; s3, collecting the used composite treatment agent, carrying out regeneration treatment, returning to the step S2 after treatment, recycling for 3 times, and then discarding; s4, evaporating and concentrating the pretreated waste acid to obtain concentrated waste acid; s5, carrying out nitric acid recovery and organic matter removal on the concentrated waste acid by using a rectification process to obtain purified sulfuric acid; and S6, recycling the purified sulfuric acid, and returning to the isooctyl nitrate esterification reaction system. According to the invention, a stepped impurity removal system is constructed through primary treatment and secondary treatment, so that the impurity removal effect is effectively improved.

The invention discloses a nitrate energetic plasticizer as well as a synthesis method and application thereof, and the synthesis method comprises the following steps: dispersing a compound 3-alkoxy-1, 2-diol propane in an organic solvent containing concentrated sulfuric acid in an ice bath, slowly dropwise adding a nitration reagent, slowly heating to a reaction temperature after dropwise adding, and reacting for 2 hours; after the reaction, pouring ice water for quenching, stirring for 30 minutes to separate an organic phase, extracting a water phase with dichloromethane, and combining the extracted organic phases; and respectively washing the organic phase with a saturated potassium bicarbonate solution and pure water for several times, removing residual moisture by using anhydrous magnesium sulfate, and carrying out reduced pressure distillation to remove dichloromethane, thereby obtaining the nitrate energetic plasticizer. The synthesis method of the aliphatic energetic plasticizer is simple, the energetic nitrate group is introduced on the basis that the aliphatic compound contains the flexible ether group, the novel aliphatic energetic plasticizer is obtained, and the aliphatic energetic plasticizer has the advantages of being low in viscosity, good in thermal stability, low in glass transition temperature and the like and is a potential application type energetic plasticizer.

The present application relates to the field of micro-channel reactor synthesis, and discloses a preparation method of isooctyl nitrate and application thereof.The preparation method of isooctyl nitrate comprises the following steps: 1) a step of contacting acid and isooctyl alcohol in one or more reaction modules; and 2) a step of purifying the reaction product to obtain isooctyl nitrate, wherein the reaction module comprises a micro-channel reactor and a tubular reactor connected in sequence, and the acid comprises sulfuric acid and nitric acid.The preparation method of isooctyl nitrate has the characteristics of high isooctyl alcohol conversion rate, high product purity, small pressure drop of the reaction system and large production capacity.

The invention relates to a safe and efficient process for the nitrate ester formation of an α,ω-C3-10alkanediol monoacylate. The process is safer to operators and allows to obtain advantageous yields on industrial scale.

The invention discloses design and synthesis of a novel nitrate modified aspirin and BOC-amino acid coupled compound with antitumor activity, and screens out an optimal candidate taking a 9 carbon chain as a Linker (compound 3e). On the basis of the structure, four BOC protected natural amino acids (BOC-L-valine, BOC-L-phenylalanine, BOC-L-tryptophan and BOC-L-methionine) are further coupled, and 9C-aspirin-BOC-L-tryptophan (a compound 7) shows the strongest activity. In-vitro experiments show that the compound 7 significantly inhibits proliferation and migration of tumor cells, and the effect of the compound 7 is superior to that of an uncoupled compound 3e. An in vivo xenotransplantation tumor model shows that the compound 7 effectively inhibits tumor growth in a dose-dependent manner. In conclusion, the antitumor activity of aspirin is remarkably improved through structural optimization of the compound 7, and a powerful candidate is provided for development of novel multi-target anti-cancer drugs. The research lays a solid foundation for clinical transformation of aspirin derivatives.

The invention discloses a treatment process for separating liquid nitrate from waste acid, and treatment equipment adopted in the treatment process comprises a temporary storage tank, a separation membrane, a liquid discharge pump, a high-position conveying assembly and a recovery tank, the treatment process comprises the following operation steps: filling the temporary storage tank with the nitrate-containing waste acid from the liquid inlet pipeline; the waste acid is discharged outwards through the separation membrane via the waste acid discharge pipeline; air is injected into the temporary storage tank, so that the nitrate layering liquid located on the upper layer is squeezed into the nitrate high liquid level pipe and discharged into the recovery tank through the liquid discharging pipe, and when the liquid level in the temporary storage tank reaches the lower end face of the nitrate high liquid level pipe, the valve on the air inlet pipeline is closed, and air injection is stopped; and 3) injecting the nitrate-containing waste acid into the temporary storage tank from the liquid inlet pipeline, and repeating the steps 2)-3) until the waste acid treatment is completed. The treatment process provided by the invention realizes separation of liquid nitrate in waste acid.

The invention relates to a nitration phase continuous flow nitration method. The method comprises the following steps: mixing a nitrating agent with a solvent 1 to obtain a nitration phase; dissolving and dispersing the raw materials through a solvent 2 to obtain a raw material phase; the nitration phase and the raw material phase are conveyed into a continuous flow reactor according to a certain flow velocity ratio, a nitration product is obtained after reaction, and continuous nitration synthesis is achieved. The nitrating agent comprises one or more of nitrate or a solid nitrating agent obtained by mixing nitrate and sulfate, grinding and sieving; nitrate, or a mixture of nitrate and sulfate, and a nitration auxiliary agent are mixed to obtain a solid nitrating agent; the fluid nitrating agent is prepared from nitrate, or a mixture of nitrate and sulfate, and water and / or a nitrating auxiliary agent; nitric acid is used as a nitrating agent; nitric acid and a nitration auxiliary agent are mixed to obtain a fluid nitrating agent; and nitrogen pentoxide. Compared with the prior art, the method provided by the invention has the advantages of no use of mixed acid, mild and controllable reaction conditions, less by-products, less amount of acid wastewater generated by the process and obvious industrialization prospect.

The present invention belongs to the technical field of preparing nitrate esters, and particularly relates to a process and device for preparing sec-octyl nitrate. The process includes: introducing a certain amount of mixed acid and sec-octanol into a raw material distribution pipeline and a microchannel reactor in the form of continuous flow through an acid pump and an alcohol pump respectively, controlling the set temperature by a heating tank, leading the crude product out of the microchannel reactor to a post-treatment receiver after nitration reaction, separating the collected ester-acid mixture, washing the organic phase, and drying to obtain the finished product. The preparation process and device of the present invention can realize the production equipment of sec-octyl nitrate, improve the synthesis efficiency and safety of sec-octyl nitrate, reduce the generation of side reaction products, and solve the problems of high process amplification cost and great difficulty in large-scale industrial production existing in the existing microchannel reactor technology.

The utility model discloses a dimethyl oxalate synthesis nitrogen source supplementing system, which relates to the technical field of chemical reaction, and is characterized in that nitric acid from the outside is input by arranging a nitric acid input pipeline, and alcohol-containing liquid and nitric oxide-containing gas from a reaction system are circularly input by arranging an alcohol-containing liquid input pipeline and a nitric oxide-containing gas input pipeline; the nitric acid enters the reaction system again, the nitric acid from the outside and the methanol from the reaction system are uniformly mixed in advance by arranging the mixer, so that the nitric acid and the methanol react with the nitric oxide from the reaction system more sufficiently, and multi-stage repeated reaction is carried out by arranging the four-stage reaction chamber; according to the invention, nitric oxide, nitric acid and methanol can be fully and effectively reacted, the loss of a nitrogen source is reduced, the outflow of nitric acid is reduced, and the treatment cost of discharged nitric acid in a subsequent working section is reduced.