169 results about "Adiponitrile" patented technology

The invention provides a hydrocyanation process for the production of adiponitrile and other dinitriles having six carbon atoms, the process comprising:

• • a) forming a reaction mixture in the presence of at least one Lewis acid, said reaction mixture comprising ethylenically unsaturated nitrites having five carbon atoms, hydrogen cyanide, and a catalyst precursor composition, by continuously feeding ethylenically unsaturated nitrites, hydrogen cyanide, and a catalyst precursor composition;
  • b) controlling X and Z, wherein X is the overall feed molar ratio of 2-pentenenitriles to all unsaturated nitriles and Z is the overall feed molar ratio of hydrogen cyanide to all unsaturated nitrites, by selecting a value for X in the range from about 0.001 to about 0.5, and a value for Z in the range from about 0.5/1 to about 0.99/1, such that the value of quotient Q, wherein

is in the range from about 0.2 to about 10, wherein 3PN is 3-pentenenitriles and 4PN is 4-pentenenitrile; and

• • c) withdrawing a reaction product mixture comprising adiponitrile;
  • wherein the ratio of the concentration of 2-pentenenitriles to the concentration of 3-pentenenitriles in the reaction mixture is from about 0.2/1 to about 10/1;
  • wherein the catalyst precursor composition comprises a zero-valent nickel and at least one bidentate phosphite ligand; and

wherein the bidentate phosphite ligand is selected from a member of the group represented by Formulas I and 11 as described herein.

The invention provides a hydrocyanation process for the production of adiponitrile and other dinitriles having six carbon atoms, the process comprising:

• • a) forming a reaction mixture in the presence of at least one Lewis acid, said reaction mixture comprising ethylenically unsaturated nitriles having five carbon atoms, hydrogen cyanide, and a catalyst precursor composition, by continuously feeding ethylenically unsaturated nitriles, hydrogen cyanide, and a catalyst precursor composition;
  • b) controlling X and Z, wherein X is the overall feed molar ratio of 2-pentenenitriles to all unsaturated nitriles and Z is the overall feed molar ratio of hydrogen cyanide to all unsaturated nitriles, by selecting a value for X in the range from about 0.001 to about 0.5, and a value for Z in the range from about 0.5/1 to about 0.99/1, such that the value of quotient Q, wherein

is in the range from about 0.2 to about 10, wherein 3PN is 3-pentenenitriles and 4PN is 4-pentenenitrile; and

• • c) withdrawing a reaction product mixture comprising adiponitrile;
  • wherein the ratio of the concentration of 2-pentenenitriles to the concentration of 3-pentenenitriles in the reaction mixture is from about 0.2/1 to about 10/1;
  • wherein the catalyst precursor composition comprises a zero-valent nickel and at least one multidentate phosphorus-containing ligand;
  • wherein the multidentate phosphorus-containing ligand is selected from the group consisting of a phosphite, a phosphonite, a phosphinite, a phosphine, and a mixed phosphorus-containing ligand or a combination of such members; and
  • wherein the multidentate phosphorus-containing ligand gives acceptable results according to at least one protocol of the 2-Pentenenitrile Hydrocyanation Test Method.

The invention discloses a rare-earth oxide modified high-selectivity catalyst for adiponitrile hydrogenation and hexylenediamine production, a preparation method and application thereof. An alumina-supported nickel-based catalyst is used as an active component, and at 25-90 DEG C and through a parallel flow precipitation process, a low-content rare-earth oxide is used for the modification. A tankreactor is adopted at the low temperature and without an alkaline reagent to carry out a reaction at the pressure of 1-9 MPa for 1-6 h so as to achieve adiponitrile catalytic conversion for high-selectivity preparation of hexylenediamine. No alkaline reagent or NH3 is added during the reaction process to inhibit side reaction of cyclization. The environmental pollution is reduced; and the catalysthas high mechanical strength, the reaction post-treatment is simple and the reaction condition is relatively mild. According to the method and in part of the embodiments, the conversion rate of adiponitrile reaches up to 100% according to set reaction parameters, and selectivity of the product hexylenediamine can reach up to 90%. The invention has good economic benefit and industrial applicationprospects.

The invention discloses a method for preparing hexamethylene diamine by direct hydrogenation of adiponitrile under alkali-free conditions. The method comprises the steps of using an alkaline earth metal oxide or rare earth metal oxide prepared by a coprecipitation method for modifying an aluminium trioxide-supported metallic nickel catalyst under a condition of no need of adding alkali or ammoniawater, directly hydrogenating an adiponitrile ethanol solution at a temperature of 60 to 200 DEG C, under pressure of 3 to 8 MPa, and obtaining high-qualityhexamethylene diamine through vacuum distillation of a resulting product. The method is suitable for using in batch tank reactors and also in continuous fixed bed reactors.

The invention relates to a rhodococcus ruber and a method for preparing 5-cyanovaleramide by utilizing the same. The strain needs oxygen, does not need power, spores and gram-positive bacteria, is already stored in the Common Microorganism Center of Chinese Microorganism Strain Storage Management Committee and has storage data of Jun. 4, 2009 and a preservation number of CGMCC No.3090. The method for preparing the 5-cyanovaleramide by utilizing the rhodococcus ruber comprises the following steps: (1) culturing seeds; (2) fermenting and culturing; (3) preparing a rhodococcus ruber suspension; (4) preparing a crude product of 5-cyanovaleramide; and (5) purifying the 5-cyanovaleramide. The invention provides a method for generating the 5-cyanovaleramide by selectively hydrolyzing adiponitrile in a rhodococcus ruber region, has high catalytic efficiency, high adiponitrile conversion rate up to 100 percent and 5-cyanovaleramide regioselectivity up to 100 percent, does not generate a side product of adipamide and simplifies the separation purification process of the 5-cyanovaleramide.

The invention relates to a method and equipment for production of adiponitrile from adipic acid, and mainly solves the problem of unstable product quality in the prior art for production of adiponitrile from adipic acid. The method employs materials of fusing adipic acid, ammonia, phosphate and a diluent. The production method is as below: mixing phosphoric acid with the diluent in a pipeline mixer; conducting neutralization of adipic acid and ammonia in a cyanation reactor; sending reaction products into the bottom of a separation tower for separation; recovering gas phase of light components from an outlet; sending the diluent recovered by a gas lifting plate into the pipeline mixer, mixing the diluent with phosphoric acid in the pipeline mixer, and sending the mixture into the cyanation reactor to dilute adipic acid; and sending a liquid phase to a scraper type evaporator. The employed equipment includes an adipic acid storage tank, an ammonia compressor, a cyanation reactor, a pipeline mixer, a separation tower, a tail gas removal tower, a phosphoric acid storage tank and a scraper type evaporator. The invention has the advantage of a good quality of the produced adiponitrile product.

The invention discloses a preparation method of hexamethylenediamine. Hexane dinitrile is used as a raw material, and a nano-nickel and magnesium oxide composite material is used as a catalyst to prepare the hexamethylenediamine through liquid phase hydrogenation. The preparation method of the hexamethylenediamine comprises the following steps: dipping a porous carrier by using nickel acetate andmagnesium nitrate aqueous solutions at different concentrations at first, and carrying out in-situ reduction to obtain an immobilized nickel and magnesium oxide based composite catalyst under different conditions; adding raw materials, the catalyst and a solvent in a reaction kettle in proportion, sealing the reaction kettle, removing air in the kettle by a hydrogen substitution method, starting aheating power supply, applying set pressure to hydrogen after the temperature in the kettle is raised to the set reaction temperature, then starting a magnetic stirrer, and beginning to time reaction; and after the reaction is finished, filtering out the catalyst, and distilling and separating under reduced pressure. The yield of a target product is high, the yield of the hexamethylenediamine isgreater than 70%, and the solvent and the catalyst are recyclable.

The invention discloses electrolyte of a lithium ion battery taking lithium titanate as cathode. The electrolyte comprises the organic solvent, lithium salt and additive dissolved in the organic solvent; the additive comprises one or the combination of the adiponitrile, butanedinitrile, 1,3-propane sultone, wherein the additive further comprises one or the combination of the cyclic acid anhydride and/or the derivate thereof, the total weight of the additive is 1-10% of the weight of the electrolyte, the weight of the cyclic acid anhydride and/or the derivate thereof, is 0.01-1% of the weight of the electrolyte. The additive comprises the cyclic acid anhydride and/or the derivate which have chemical reaction with the water in the battery, the combination water in the lithium titanate material, the water, the hydroxy and other groups for generating one component of the electrolyte, the defect that the water cannot be removed totally in the conventional vacuum baking process is compensated. The catalytic reaction for the hydroxy can be effectively avoided while having reaction with the Ti-OH bond on the surface of the lithium titanate particle, and the high temperature storage performance and the high temperature circulation performance of the lithium titanate battery are improved.

The invention relates to a preparation method of adiponitrile. The preparation method comprises the following steps: firstly performing a reaction on adipic acid and ammonia at 155-200 DEG C to produce diammonium adipate, and then dehydrating under a catalytic reaction of phosphoric acid or ammonium phosphate to produce adiponitrile; a product can be further separated in a separation tower. The reaction is performed on the adipic acid and the ammonia gas at the low temperature of 155-200 DEG C to produce H4NOOC(CH2)4COONH4 first, and then high-temperature cyanation is performed, so that the opportunity of producing a by-product and a coke from the adipic acid at high temperature is effectively avoided, not only the yield is increased by 3-5%, but also the operation cycle of a production device is prolonged by 30-60 days, and the production per unit time is increased. Liquid phosphoric acid is used as a catalyst, firstly ammonium salt of the phosphoric acid is produced, and the ammoniumphosphate can be mixed with ammonium salt of the adipic acid very well, so that the catalytic performance is improved better and the selectivity of the adiponitrile is increased by more than 2%.

The invention discloses a method for activating an adiponitrile hydrogenation catalyst. The method is characterized in that the catalyst is a modified raney nickel catalyst and is activated by the method comprising the following steps: preparing a mixing solution from iron, chromium, molybdenum, bismuth, manganese or tungsten soluble salts and NaOH respectively; slowly adding the modified raney nickel catalyst and ammonium salt; heating with microwave and reacting, and then washing; the modified raney nickel catalyst is prepared by the method comprises the following steps: grinding nickel-aluminum alloy into powder; adding to a mixing solution to dissolve part of aluminum, wherein the mixing solution is prepared through NaOH, ammonium salt and ammonium hydroxide in certain ratio; washing with deionized water and absolute ethyl alcohol; adding the powder to the mixing solution consisting of ferric nitrate and a modifier under a microwave condition and reacting to obtain a solid; drying and roasting the solid; and then charging hydrogen and reducing to obtain the modified raney nickel catalyst. With the adoption of the method for activating the adiponitrile hydrogenation catalyst, the prepared catalyst is relatively large in specific surface area, loss of the modifier is small, and high conversion rate of adiponitrile and high selectivity of hexamethylenediamine are achieved in the adiponitrile catalytic hydrogenation process.

The invention relates to an electrolyte and a lithium ion battery comprising the same. The electrolyte comprises an organic solvent, a lithium salt, vinylene carbonate, fluoroethylene carbonate and a combined additive, wherein the combined additive comprises the following raw materials by percentage: 0.1%-7% of propane sultone, 0.1%-7% of ethylene sulfate and 0.1%-9% of adiponitrile on the basis of total weight of the electrolyte. The electrolyte provided by the invention is applied to the lithium ion battery, so that the initial efficiency, the cycle performance, the high-temperature storage performance, the overcharge resistance performance and the safety performance of the lithium ion battery at high voltage of above 4.4V can be greatly improved.

The invention discloses an electrolyte for a lithium ion battery. The electrolyte comprises the following components in percentage by weight: 10-15% of lithium hexafluorophosphate, 0.1-0.5% of hexamethylene diisocyanate, 0.5-2% of vinylethylene carbonate (VEC), 0.5-5% of fluoroethylene carbonate (FEC), 10-20% of ethylene carbonate (EC), 25-50% of diethyl carbonate (DEC), 10-20% of ethyl methyl carbonate (EMC), 3-5% of 1, 3-propane sultone (PS), and 1-3% of adiponitrile (ADN). The matching ratio of the components in the electrolyte is optimized, and the high-temperature type additive which refers to the hexamethylene diisocyanate is chosen, so that the storage performance of the lithium ion battery under a high temperature can be improved; and meanwhile, the additives, such as the FEC, the VEC and the like are reasonably utilized, so that the problem of relatively bad low-temperature performance caused after the HMDI is added can be effectively relieved.

The invention discloses an electrolyte of a power lithium ion secondary battery, which is prepared from an electrolyte, a main solvent and an additive according to certain mass percents; the electrolyte of the invention is characterized in that the electrolyte comprises 5-15% of lithium hexafluorophosphate and 1-10% of lithium bis(oxalate)borate; the main solvent comprises 25.0%-35.0% of dimethyl carbonate (DMC), 5.0%-15.0% of ethyl methyl carbonate (EMC), 3.0%-10.0% of ethylene carbonate (EC), and 2.0%-8.0% of propylene carbonate (PC); the additive comprises 1%-3% of ethylene sulfite (ES), 1%-3% of vinylene carbonate (VC), 0.5%-2.0% of 1,3-propane sultone (PS), 0.1%-0.5% of anisole, 0.5%-2.0% of biphenyl (BP), 0.01%-2% of adiponitrile, 0.5%-2.0% of gamma-butyrolactone (GBL), and 0.5%-2.0% of cyclohexylbenzene (CHB). The electrolyte of the invention can significantly improve conductivity, wettability, and high temperature circularity, thus enlarging the application scope of the electrolyte.

The invention provides a preparation method of 3-pentenenitrile and a preparation method of adiponitrile. The preparation method of 3-pentenenitrile comprises the following steps: 1, performing the hydrocyanation reaction on raw material mixed solution of butadiene and hydrocyanic acid under the action of a catalyst so as to obtain a first mixture containing the 3-pentenenitrile; and 2, carrying out separation on the first mixture to obtain the 3-pentenenitrile, wherein the catalyst is a coordination complex consisting of monodentate phosphine, bidentate phosphine and zero-valent nickel. By adopting the method, the 3-pentenenitrile can be effectively, efficiently and economically prepared by using the butadiene and the hydrocyanic acid as the raw materials; the integral process is safe and reliable; the flow is simple; and moreover, production cost and equipment investment can be obviously reduced.

The invention discloses an apparatus and a method for preparing adiponitrile by electrolyzing acrylonitrile assisted by electro-active microbes. The apparatus comprises a microbe electrolytic tank, a data acquisition system and a recording unit, wherein an anode electrode and a cathode electrode of the microbe electrolytic tank are made of electrically inert materials; the anode electrode and the cathode electrode are connected through a titanium wire, a constant potential rectifier and a resistor; the data acquisition system is connected with the resistor in parallel; and the recording unit is connected with the data acquisition system. The method comprises the steps of organic materials are metabolized by electro-active microbes in an anode chamber of the microbe electrolytic tank to produce electrons and protons; the produced electrons are transferred to the anode electrode directly or indirectly and then transferred to the cathode electrode along an external circuit under the effect of an applied voltage; at the same time, H<+> ions pass through an ion exchange membrane and are migrated to a cathode chamber of the microbe electrolytic tank; H<+> ions, the electrons and acrylonitrile are combined on the surface of the cathode electrode with relatively high hydrogen evolution over potential to generate adiponitrile. The apparatus and the method have the advantages of low energy consumption, no corrosions to the anode electrode, etc. Besides, the apparatus and the method can reduce discharge of organic wastes.

The invention discloses a hydrogenation catalyst, and a preparation method and application thereof, belonging to the field of hydrogenation of adiponitrile. The hydrogenation catalyst comprises the following components in percentage by mass: 60-90% of active component, 1-30% of aid and 1-10% of at least one metal selected from Group IIA metals. The preparation method comprises the following steps: preparing a mixed solution from the components, putting the mixed solution in an 80-110-DEG C environment, and performing reaction for 1-8 hours to obtain the hydrogenation catalyst. The hydrogenation catalyst is applied to reduction reaction. The hydrogenation catalyst has the advantages of small particle size, uniform particle size distribution (15-18nm), large specific area (up to 25-30 m<2>/g), high hydrogenation activity, favorable selectivity, low price, simple preparation technique, easy operation process and low requirements for processing equipment, and can be easily separated from the product after the reaction finishes. The hydrogenation catalyst is applicable to tank reactors, fluidized bed reactors and fixed bed reactors, and thus, has favorable adaptability to equipment.

The invention discloses a preparation method and application of a nitrogen-doped activated carbon supported alkali metal modified nickel-based catalyst. The preparation method includes the steps that firstly, acid activation or acid modification is conducted on a wooden charcoal material, nitrogen doping treatment is conducted on the wooden charcoal material, and then the wooden charcoal material is impregnated and supported with nickel and alkali metals. The nitrogen-doped activated carbon supported alkali metal modified nickel-based catalyst is applied to an adiponitrile hydrogenation process and can have high activity and high overall selectivity on 6-aminocapronitrile and hexamethylenediamine under relatively mild reaction conditions. Usage of a large number of precious metals serving as active components is avoided, equipment is not corroded (a large amount of additional ammonia or alkali metal hydroxide for inhibiting the formation of by-products is not needed), the cost is low, the catalyst is friendly to the environment, the preparation process of the catalyst is simple, the used active charcoal material is cheap and easy to obtain, and the preparation method is simple and has a very good application prospect.

The invention discloses a solid phosphorus acid catalyst for producing adiponitrile and a preparation method of the solid phosphorus acid catalyst. The preparation method of the solid phosphorus acid catalyst comprises the steps as follows: diatomite is impregnated in a phosphoric acid and sulfate mixed solution, and a carrier is separated through centrifugation after impregnation balance, and then drying and roasting are performed, wherein the concentration of phosphoric acid is 55wt%-95wt%, the concentration of sulfate is 15wt%-25wt%, the roasting temperature is 300-700 DEG C, sediment is cooled and then subjected to preforming, particles between 10 meshes and 50 meshes are screened, and the solid phosphorus acid catalyst is formed. One novel green catalyst is developed for production of adiponitrile with an adipic acid liquid phase method, and the catalysis effect is improved while various defects caused by traditional catalysts are overcome.

The invention relates to a method for electrosynthesis of adiponitrile by using a dimensionally stable anode. The method comprises the following steps of: carrying out electrosynthesis of the adiponitrile in a non-diaphragm type electrolytic bath by utilizing titanium as a substrate, utilizing the dimensionally stable anode coated with oxides, such as ruthenium, iridium, tantalum and the like as an anode and utilizing plumbum or cadmium as a cathode; introducing a direct current of 500 A.m-2-3,000A.m-2 at the temperature of 20-60 DEG C for electrolysis; and maintaining the flow rate of interelectrode electrolytes to be more than 1m.s<-1>, wherein the electrolytes contain 0.5-7% by mass of acrylonitrile, 5-20% by mass of potassium phosphate, sodium phosphate, acid type potassium phosphate or acid type sodium phosphate as supporting electrolytes, 0.1-5.0% by mass of buffer, 0.1-10.0% by mass of guiding ion source quaternary ammonium salt and the balance of water, the pH value of the electrolyte is 6-10. An organic phase containing a product of adiponitrile, a by-product of propionitrile and a raw material AN (Acrylic Nitrile) which does not participate in the reaction is generated from electrolysis. The adiponitrile and the propionitrile are obtained from the organic phase through rectification. The method overcomes the defect of easy corrosion of the anode in the electrolysis, the yield of the adiponitrile reaches more than 80%, and the current efficiency is more than 75%.