171 results about "Triethylamine hydrochloride" patented technology

The manufacture method of a kind of zirconia fibre cotton relates to the field of resistance of fire fibre material. We compose van-style acetamide acetone zirconium polymer according to chloridze zirconia, acetamide acetone and three-ethylamine. We use methanol as the dilute impregnant, we mix round them to let hloridize zirconia, acetamide acetone and three-ethylamine react at 40-20 deg.C, and we can receive poly-acetamide acetone zirconium van-substance. Four-hydrogen furan filtrate and remove the outgrowth hydrochloric three-ethylamine. The offspring dissolve in the filature liquid made of methanol. After centrifugal swing, we can receive van-substance fibre. After we do special hear treatment, the zirconia fibre cotton we receive has the characteristic of good filature ability, high content of zirconium, equality andclarity and jarles capability. It can be used as industrial stove, roomage fusion stove, atomic energy reactor and the high temperature heat insulation material used in aviation and military. The material of the invention cost low, the method is easy, the impregnant can be recycled, the preparation of fibre cost low.

The invention relates to a method of preparing full-stable and cubic-phase zirconia crystal fibers, which mainly comprises the following steps: using zirconium oxychloride, acetylacetone and triethylamine as main raw material and using ethanol as diluent solvent to directly react at a temperature of 0 DEG C to 50 DEG C under a stirring condition so as to generate an organic polymer solution comprising zirconium; evaporating the ethanol and using acetone as solvent to dissolve soluble substances and filter and remove an undissolved substance of triethylamine hydrochloride; recycling the acetone, dissolving the obtained products and yttrium salt to the ethanol to prepare a spinning solution which is centrifugally flung at a high speed to obtain organic polymer fibers comprising zirconium; and carrying out heat treatment in a special atmosphere and ultra-high temperature treatment of the organic polymer fibers comprising zirconium. The invention has simple preparation technology and can recycle the solvent, and the prepared crystal fibers have single ingredients, high purity and stable high-temperature performance and can be used in a range from 1700 DEG C to 2150 DEG C for a long time.

The producing method of two-oxidation titanium fibre belongs to function fibre material technology scopes. Compose poly-acetamide acetone titanium to be the van-substance. Let chemic dosage of four-chloridize titanium, distilled water, acetamide acetone and three-ethylamine dilute in methanol respectively. Mix them and react when mixing round at 0-25 deg.C. Compose poly-acetyl acet, titanium. Remove hydrochloric three-ethylamine by using four-hydrogen furan. Dissolve poly-acetyl acet, titanium in methanol to make filature liquid. Obtain van-substance short fibre by using acentric swing method. Obtain van-substance long fibre by using dry filature method. And we can obtain two-oxidation titanium fibre by using high pressure or normal pressure vapor heat treatment technique agglomeration. The intension of extend of this invention is 100 MPa-1.2GPa. The diameter is 3um-20um. The one-thread series length is 1 cm-50 cm or higher than 1 m. The crystal diameter is 5 nm-100 nm. The appearance is two-oxide ation short fibre or consecutive fibre with titanium droff-titanium-mine posture or rutile posture or coexistence.

The invention provides a method for preparing AKD by serialization. The method includes the following steps: reaction of acyl chloride and tertiary amine is carried out, acyl chloride in formula ratio is divided into two or three parts, each part is 10-90% of the formula ratio, the rest part of acyl chloride is added in times after 30-300 seconds, triethylamine in formula ratio and first part of acyl chloride are simultaneously, respectively and continuously added at the front end of a reactor; material is continuously fed into a hybrid reactor from different feeding holes by virtue of a plurality of metering pumps, the material is subject to hybrid reaction in the hybrid reactor by stirring, cutting and malposition moving, and the temperature of material is controlled; the material is remained in the reactor, discharged from the outlet of the reactor and enters into a continuous extractor, and meanwhile diluted hydrochloric acid is continuously added into the extractor, is dispersed with reaction product to form uniform mixed solution and then enters into a slope precipitator, separation of oil phase and water phase is carried out, the oil phase is discharged from the upper outlet, and the water phase is discharged from the lower outlet; and the oil phase is namely the AKD, and the water phase is triethylamine hydrochloride solution.

The invention discloses a method for synthesizing vinylene carbonate, and the method mainly comprises the following steps: (1) chlorine gas is introduced into the raw material of ethylene carbonate in ultraviolet light condition, thus synthesizing chlor-ethylene carbonate; (2) taking mixture of ester, ether and hydrocarbon as the organic solvent, the chlor-ethylene carbonate which is obtained in the step (1) produces elimination reaction with triethylamine, thus eliminating hydrogen chloride and generating the vinylene carbonate; and (3) the mixed product obtained in the step (2) is distilled and purified after filtration. By adopting the mixed solvent of ester, ether and hydrocarbon, the reaction product is easily isolated from triethylamine hydrochloride, thus increasing the yield and the production efficiency; and BHT can be used as a polymerization inhibitor in the reaction process, thus controlling the polymerization of the vinylene carbonate effectively and increasing the yield.

The invention relates to a method for preparing cyclohexylbenzene by benzene and cyclohexene through alkylation reaction, comprising the main step that under the condition with a catalyst, target substance is prepared by the benzene and the cyclohexene through the alkylation reaction; the invention is characterized in that the catalyst is imidazole ionic liquid or triethylamine hydrochloride ionic liquid. The invention overcomes the defects that the catalyst in the prior art can not be repeatedly used or the reaction activity decreases after repeated usage.

The invention belongs to the field of wet metallurgy and in particular discloses a compound leaching agent for preventing landslide in the process of leaching weathering crust deposit type rare earth ore in situ. The compound leaching agent consists of a mixed aqueous solution of an organic amine salt anti-swelling agent, a leaching agent and a pH regulator, wherein the concentration of the organic amine salt anti-swelling agent is 1-15g/L; the concentration of the leaching agent is 5-30g/L; the pH value of the mixed aqueous solution is regulated to be 4.0-6.0 by using the pH regulator. The compound leaching agent is preferably any one of dimethylamine hydrochloride, di-n-propylamine hydrochloride, diethylamine hydrochloride and triethylamine hydrochloride. Due to the addition of the anti-swelling agent, the compound leaching agent has the capacity of well preventing swelling of clay minerals, the rare earth leaching effect is not influenced, the leaching agent has the functions of leaching and preventing swelling, and landslide is effectively avoided in the process of leaching the weathering crust deposit type rare earth ore in situ.

A method for recovering triethylamine from triethylamine hydrochloride aqueous solution comprises allowing calcium oxide and the triethylamine hydrochloride to react, and distilling at 50-150 DEC C to obtain the triethylamine; adding the calcium oxide into the collected triethylamine, refluxing under heating to remove water, and distilling to collect the triethylamine having water content smaller than 0.5%, distilling to obtain the triethylamine, separating solid from a turbid aqueous solution residual in a reaction kettle, adjusting the pH value of the aqueous solution to 7 with hydrochloric acid, and removing water to respectively obtain calcium chloride hexahydrate, calcium chloride dehydrate and anhydrous calcium chloride; and allowing the calcium oxide after drying the triethylamine and the triethylamine hydrochloride to react to obtain the triethylamine. Compared with the prior method for recovering the triethylamine from the triethylamine hydrochloride aqueous solution, the method has the advantages of simple operation, low price, high recovery rate, and no three wastes discharge.

The invention relates to a preparation method of combustion inhibitor containing P-S, which includes the steps: (1) under the nitrogen gas atmosphere, adding triethylamine hydrochloride and anhydrous aluminium chloride, mixing; (2) adding benzene into refluxing liquid of PCl3 and [Et3NH]Cl-2AlCl3 for refluxing reaction; vacuum distilling, and then adding sulphur powder in batches for continue reaction; adding petroleum ether and stirring, separating and collecting petroleum ether phase on upper layer, washing, drying; pressure reducing and steaming petroleum ether; collecting distillate; dispersing pentaerythritol and pyridine in carrene, dropping sulfo-phenylphosphono with stirring for refluxing reaction, after the reaction ends, rotary steaming, water washing and recrystallizating. The combustion inhibitor provided the invention has good char formation.

The invention discloses a method for treating glyphosate mother solution, which comprises the following steps of: adding aqueous solution of calcium hydroxide into the glyphosate mother solution to regulate pH until the solution is alkaline and make triethylamine hydrochloride in the mother solution generate triethylamine simultaneously; adding the treated glyphosate mother solution into a distillation tower for distillation, and collecting 40 to 100 DEG C fractions on the top of the tower; adding a dehydrating agent into the fractions on the top of the tower to obtain the triethylamine; and adding hydrochloric acid into the mother solution at the bottom of the tower to regulate the pH until the solution is neutral, performing solid-liquid separation and treating and discharging separatedwaste water. The process is simple and high-efficiency; the recovery rate of the triethylamine is over 98.5 percent; the chemical oxygen demand (COD) of the discharged waste water is less than 500mg/L, total phosphate (TP) is less than 1mg/L and ammonia nitrogen is less than 15mg/L; the zero emission of the waste water is basically realized; and the method has great environmental benefit and economical benefit.

The invention relates to a flame retardant, a preparation method and purposes thereof. The flame retardant is called O-alkyl acrylamide dialkyl thiophosphate. The preparation method is that: 1mol new distilled N- hydroxyalkyl acrylamide is dissolved in 500ml dry aether and poured into a 1000ml four-neck reaction flask with a constant pressure funnel, a refluxing condensing tube and a magnetic stirrer, and 1.05mol distilled triethylamine is added, and the reaction temperature is kept at 0-50 DEG C, then 1mol distilled sulfur dialkyl phosphoryl chloride is dripped into the reaction flask through the constant pressure funnel and the time of dripping is controlled for 1-6h; reaction is kept for 10-48 hours under room temperature, then the reaction is stopped and filtration is made to take out triethylamine hydrochloride, the filtrate is washed with 5 percent sodium hydroxide solution, then is washed with distilled water, and distillation is carried out to remove the aether and water, finally drying is carried out with anhydrous magnesium sulfate so as to obtain the O-alkyl acrylamide dialkyl thiophosphate. The flame retardant of the invention is particularly applicable to be used as a comonomer to prepare flame retardant Orlon.

A synthetic method of a superhigh temperature resistant zirconium carbide ceramic precursor belongs to preparation methods of ceramic precursors. The synthetic method includes firstly, dissolving 6.44g zirconium oxychloride in 50 mL absolute methanol, stirring the mixture at a room temperature for dissolving, subjecting the mixture to ice bath for cooling, dropwise adding 2.4g-3.47g saligenin, finally dropwise adding 4.24g triethylamine at a dropping speed of 1 droplet per second, and subjecting the mixture to magnetic stirring in the process of the dropping adding; after the dropping adding, removing the ice bath and stirring the mixture at a room temperature for 4 hours; then subjecting the mixture to rotary evaporation for 10 minutes to evaporate solvents, adding 50 mL tetrahydrofuran, stirring the mixture at a room temperature for 2 hours, and performing suction filtration to remove a precipitation of triethylamine hydrochloride; subjecting the mixture to rotary evaporation for 15 minutes to evaporate the solvents of colatuie, adding 100 mL hexyl hydride, stirring the mixture at a room temperature for 12-48 hours, performing filtration to obtain a pale yellow precipitation, and subjecting the pale yellow precipitation to vacuum drying for three hours to obtain the zirconium carbide ceramic precursor. The synthetic method of the superhigh temperature resistant zirconium carbide ceramic precursor has the advantages that the even dispersing of modular zirconium components in precursor reins is achieved, the solidification group saligenin are contained in the ceramic precursor so that crosslinking solidification is facilitated, the synthesis temperature is low, the reaction speed is rapid, and the toxicity of solvents is small.

The invention belongs to drug synthesis, particularly relates to the main ring of Sartan drug for the treatment of the hypertension i.e. 5-(4'-formyl biphenyl-2-base)-1H-tetrazole. The preparation method comprises the following procedures, bromination, esterification, cyclization, hydrolysis and oxidation. Utilizing the triethylamine hydrochloride to serve as the catalyst, the method of the invention inhibits the side reaction, promotes the purity and the yield of the product, avoids the residue of the poisonous matter in the drug intermediate, reduces the waste discharge, realizes the clean production and protects the environment.

The invention discloses an aluminum ion battery. Electrolyte is ionic liquid composed of triethylamine hydrochloride and aluminum chloride according to the mol ratio of 1 to (1.4 to 1.6); a positive electrode is a graphene foam positive electrode material. According to the aluminum ion battery disclosed by the invention, mostly, triethylamine hydrochloride used in the aluminum ion battery is an industrial waste material, is easy to obtain and low in cost, so that the triethylamine hydrochloride is an environment-friendly and cheap raw material. The power density and energy density of the aluminum ion battery are ensured, and the cut-off voltage and specific capacity of the battery are improved by utilizing the ionic liquid; meanwhile, the efficiency is ensured, so that the safety and energy storage performance of the battery are improved.

The invention discloses a method for reducing COD (chemical oxygen demand) of permanent violet process wastewater and an application of the method and belongs to the technical field of pigment wastewater treatment. The method comprises the following steps: firstly, process wastewater is collected and treated in a classified manner according to specific pollutants of the wastewater: a nekal-bx-containing nitride washing wastewater is subjected to alkali regulating treatment, a flocculating agent is added for coagulating sedimentation, and an anionic surfactant is removed; layered wastewater produced through solvent o-dichlorobenzene recovery is subjected to alkaline hydrolysis and stripping; high-concentration wastewater containing triethylamine hydrochloride at a front section is separated from finished washing wastewater and subjected to alkali regulation and distillation, and triethylamine is recovered; secondly, the three parts of treated wastewater are mixed with other acidic wastewater for iron-carbon micro-electrolysis and Fenton oxidation coupled reinforced treatment. Classified collection and quality-divided treatment are performed according to features of the wastewater pollutants, the treatment process is safe and environment-friendly, wastewater treatment is targeted, refractory organics are removed to a greater extent, and the COD and total nitrogen content of the wastewater are reduced.

The present invention is technological process of preparing bisphenol monoacrylate compound as oxidant with bisphenol compound, acrylic acid and phosphorus oxychloride as materials, triethylamine as acid absorbent and aliphatic hydrocarbon as solvent, and through acyl chlorination and esterification in a reactor. The technological conditions include the molar ratio between bisphenol compound and acrylic acid of 1 to 1.05, the molar ratio between acrylic acid and phosphorus oxychloride of 3 to 1.05, the molar ratio between phosphorus oxychloride and triethylamine of 1 to 3.5; reaction temperature of 63-66 deg.c and reaction time of 150-155 min. After reaction, the resultant is filtered to eliminate solid triethylamine hydrochloride, the filtrate is cooled to re-crystallize to produce white crystal product of smelting point 117.5-18.6 deg.c. The present invention is simple, and has high bisphenol monoacrylate compound yield and low material consumption.

The present invention discloses a method for synthesizing MPC using a one-pot method, comprising the following steps: step 1. dissolving phosphorus oxychloride in acetonitrile, slowly adding a mixture of ethylene glycol and triethylamine dropwise to the acetonitrile at -10 DEG C, stirring for 30 minutes at -10 DEG C, then stirring for one hour at room temperature, cooling the reaction solution to -10 DEG C; and step 2. slowly adding a mixed solution of hydroxyethyl methacrylate (HEMA) and triethylamine dropwise at -10 DEG C, stirring for three hours at -10 DEG C, cooling to -20 DEG C, removing triethylamine hydrochloride by filtration under a nitrogen atmosphere, feeding trimethylamine to a mother liquor, sealing a reactor, heating to 60 DEG C, keeping at the temperature and stirring for 26 hours continuously, evaporating solvents at 20 DEG C after cooling, adding acetone to give a solid powder, washing with acetonitrile, and filtering in presence of nitrogen. The method for synthesizing MPC using the one-pot method of the present invention is simple in operation, and helps to save a lot of inputs of devices and raw materials, reduce costs and provide a good direction for industrial production of MPC monomers.

The invention discloses a preparation method of 2, 3, 5-trimethyl benzoquinone (TMBQ), which comprises the following steps of: (1) mixing CuCl2 and/or CoCl2, ferric chloride and triethylamine hydrochloride, evenly stirring and preparing a composite catalyst; (2) dissolving trimethylolpropane (TMP) in an organic solvent and preparing a TMP organic solvent solution; and (3) adding the prepared composite catalyst into the TMP organic solvent solution, stirring, evenly mixing, heating until backflow, dropwise adding a hydrogen peroxide aqueous solution and then carrying out reaction for 2-8hours at the temperature of 20-80 DEG C, and cooling the reaction solution to room temperature; and finally obtaining the TMBQ product after separating and purifying. The preparation method of the 2, 3, 5- TMBQ adopts TMP catalytic oxidation for one-step synthesis of TMBQ, and is a green technology, the oxidizing agent and solvent which are adopted by the preparation method have the advantages of being low in toxicity and harmless, the composite catalyst has high activity, and the transformation rates of the TMP and the selectivity of the TMBQ are high.

The invention relates to a preparation method of an irbesartan isomer and an irbesartan condensation compound isomer as an irbesartan intermediate. The method comprises the following steps: 1) a phase transfer catalyst and an organic solvent are added to an irbesartan ring compound hydrochloride and biphenyl bromide, a sodium hydroxide solution is added, a reaction liquid is filtered after sufficient reaction of the raw materials, a filter cake is subjected to column chromatographic separation, and the irbesartan condensation compound isomer is obtained; 2) triethylamine hydrochloride, sodium azide and an organic solvent A are added to the irbesartan condensation compound isomer, the materials are heated to 100-130 DEG C and reacted, the sodium hydroxide solution and an organic solvent B are added, the mixture is stirred, left to stand and subjected to organic layer removal, hydrochloric acid is added to an aqueous-layer solution to regulate pH to 3.5-6.0, the solution is stirred and filtered, a filter cake is subjected to recrystallization with an organic solvent C or subjected to column chromatographic separation, and the irbesartan isomer is obtained. The irbesartan isomer impurity and the irbesartan intermediate prepared with the method have higher purity and lower energy consumption and cost. Meanwhile, the preparation method is simple to operate and environment-friendly and has important value in irbesartan production and research.

The invention relates to a recovering and applying method of triethylamine in an acylation liquid for preparing levofloxacin 1 by a 2,3,4,5-tetrachloro benzoyl chloride acxylation method, belonging to the technical field of fine chemicals. The method is realized by the following steps: 1) filtering the acylation liquid in the process of preparing the levofloxacin by using the 2,3,4,5-tetrachloro benzoyl chloride acxylation method, so as to separate out the triethylamine, wherein the filtrate is an acylated mother liquid, and a filter cake is triethylamine hydrochloride; and 2) adding liquid alkaline to regulate the filter cake triethylamine hydrochloride to alkalinity, so that the triethylamine hydrochloride is converted into the triethylamine hydrochloride to be separated out, extractingwith an organic solvent, dehydrating and converting for synthesis. The triethylamine recovering method is simple to operate, rectification is not needed, and the recovery rate is high and reaches above 93% which is equivalent to the fact that about 35 kg of triethylamine is just added in production of 1 ton of levofloxacin 1, and for expensive triethylamine, production cost is greatly reduced.

The invention discloses a treatment process of glyphosate mother solution. The glyphosate mother solution is the remaining mother solution obtained after separating glyphosate bulk drug from a system when an acidolysis reaction is over during a process of producing the glyphosate bulk drug by a dialkyl phosphate method. The treatment process of the glyphosate mother solution comprises the following steps: containing the glyphosate mother solution in a concentration device; separating to eliminate most of water under a depressurization condition to separate the glyphosate bulk drug dissolved in the mother solution; standing for layering, wherein, an upper layer is triethylamine hydrochloride and a lower layer is aqueous solution containing the glyphosate; combining the solution of the lower layer with the glyphosate for the concentration treatment process of next batch; neutralizing the triethylamine hydrochloride of the upper layer with alkali to adjust pH value to 8-13; rectifying the triethylamine of the upper layer and returning to a glyphosate synthesis procedure for recycle. The solution of the lower layer is distilled to recover a small amount of the triethylamine hydrochloride, and then discharged after biochemical treatment or used for preparing 10% glyphosate solution. The treatment process is suitable for treatment of the glyphosate mother solution.

The invention provides a method for preparing losartan shown in a formula (I). The method comprises the following steps: reacting 2-butyl-4-chlorine-5-(hydroxymethyl)-1-{[(2'- cyano-group) xenyl-4-group]methyl} imidazole and natrium azide and triethylamine hydrochloride shown in a formula (II) in toluol; regulating the obtained reaction liquid by alkali to separate organic layers; adding a reducing agent into the collected liquid; regulating the obtained reaction liquid by acid to obtain losartan solid; and if required, refining the losartan solid by isopropyl alcohol. The method has the advantages of high yield, high purity of the losartan, low cost, little environmental pollution and suitability for industrialized production.

The invention discloses two preparation methods of piperazine ethane sulfonic acid derivatives. In the early stage of feeding, the reaction is initiated by pre-heating, and heating is carried out after the system is self-heated to a certain degree by reaction, so as to effectively control side reaction of 2-hydroxyethyl piperazine and 2-chloroethane sulfonic acid sodium salt, so that the reactioncan be carried out relatively thoroughly. By reducing the way of adding NaOH solution, the generation of NaCl in the reaction system is reduced, and then triethylamine hydrochloride soluble in water and ethanol is formed by forming salt with triethylamine, which can be directly removed from the system, thus reducing the way of desalting using ion exchange resin; by directly adding the mixed solution of ethanol to the water of the original reaction system for recrystallization, and further using ethanol-water mixed solution in the amount of water added, recrystallization is performed, so as toeffectively reduce the residue of inorganic salts, and the final product has relatively high purity.

The invention discloses a high-thermal stability two-component organic gel. The high-thermal stability two-component organic gel is a mixed system which is prepared from N<1>,N<3>,N<5>-tris(2-ethylhexyl)phenyl-1,3,5-triformamide serving as a first gel factor, triethylamine hydrochloride serving as a second gel factor and a low-polarity organic solvent. According to the two-component organic gel disclosed by the invention, a porous three-dimensional reticular super-molecular structure is constructed through a synergistic effect between the first gel factor and the second gel factor; the formedorganic gel has high thermal stability, namely, gel-solution phase transition.