- Urea-based blend composition and method for the manufacture thereof
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The invention relates to a solid, particulate, urea-based blend composition comprising a urea-based compound in particulate form, one or more components in particulate form, selected from the group of nitrates, phosphates, sulphates and chlorides, and a urease inhibitor of the type phosphoric triamide, in particular N-(n-butyl) thiophosphoric triamide (nBTPT), wherein the urea-based blend composition is further characterized in that it comprises one or more reactive alkaline or alkaline-forming inorganic or organic compounds. The composition according to the invention has been stabilized against the degradation of a urease inhibitor of the type phosphoric triamide, in particular N-(n-butyl) thiophosphoric triamide (nBTPT). The invention further relates to a method for the manufacture of the claimed solid, particulate, urea-based blend composition.
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- Continuous preparation method and preparation device of N-n-butyl thiophosphoric triamide
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The invention relates to a continuous preparation method and a preparation device of N-n-butyl thiophosphoric triamide. The preparation method comprises the following steps: (1) adding a thiophosphoryl chloride toluene solution and n-butylamine into a micro-channel reactor for substitution reaction to obtain an N-n-butyl dichloro thioxophosphamide toluene solution, treating the N-n-butyl dichlorothioxophosphamide toluene solution with an anion exchange resin, and feeding the treated N-n-butyl dichloro thioxophosphamide toluene solution into a storage tank; (2) adding the solution in the storage tank and ammonia gas into a tubular reactor for reaction to obtain an N-n-butyl thiophosphoric triamide toluene solution; and (3) carrying out extraction washing, organic phase concentration recrystallization, separation and drying on the obtained solution to obtain the high-purity N-n-butyl thiophosphoric triamide. According to the continuous preparation method and the preparation device disclosed by the invention, the continuity of the production process of the N-n-butyl thiophosphoric triamide is realized, the defect of intermittent operation of a kettle type reactor is avoided, the process is simplified, the reaction selectivity is improved, and the purposes of clean production, shortening of the production period and reduction of the production cost are achieved.
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Paragraph 0039; 0041-0044; 0046-0048; 0050-0052; 0054-0056
(2020/04/17)
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- A continuous reaction synthesis N - alkyl thio phosphoric triamide
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The invention discloses a method for synthesizing N-alkylthiophosphoryl triamide through a continuous reaction. The method comprises the following steps: 1, mixing thiophosphoryl chloride with an organic solvent, pre-cooling the obtained mixture in a heat exchanger to -5-0DEG C, mixing the material with an aminated compound pre-cooled to -5-0DEG C, and reacting the obtained mixture in a micro-reactor to obtain N-alkylthiophosphoryl dichloride at the outlet of the reactor; and 2, allowing N-alkylthiophosphoryl dichloride to directly enter an ammoniation reactor, carrying out an ammoniation reaction on N-alkylthiophosphoryl dichloride and ammonia gas, and post-processing after the ammoniation reaction is completed to obtain N-alkylthiophosphoryl triamide. N-alkylthiophosphoryl triamide is synthesized through a micro-reaction technology with high mass transfer and heat transfer efficiency, so conversion of intermittence to continuity is realized, the operating step is simplified, and the reaction yield is improved.
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Paragraph 0033; 0035; 0036; 0037; 0045; 0048; 0050
(2017/08/25)
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- Synthesis method for urease inhibitor and application of urease inhibitor
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The invention relates to a synthesis method for urease inhibitor and application of the urease inhibitor and belongs to the technical field of fertilizer synergists. The synthesis method includes the steps that n-propylamine/n-butylamine and phosphorus oxychloride serve as initial raw materials and are mixed with a solvent respectively to form two mixtures; an acid-binding agent is added to the two mixtures, the first temperature process temperature is adjusted to 10-50 DEG C, pressure is controlled to 0-0.5 MPa, after a first temperature process reaction, the temperature is reduced to 0-30 DEG C, and ammonia gas is introduced for a second temperature process reaction; a crude product is obtained after the second temperature process reaction is completed, and the finished product is obtained after the crude product is layered and then treated. The synthesis method is applied to preparation of the urease inhibitor and special urea and has the advantages of being short in processing flow, fewer in product impurities, high in utilization rate and good in heat stability, achieving continuous production and the like.
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Paragraph 0062; 0063
(2017/01/19)
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- Production method of N-alkyl substituted phosphoric triamide
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The invention relates to a production method of N-alkyl substituted phosphoric triamide. In an organic solvent, liquid ammonia reacts with alkyl amino phosphorodichloridate. The production method further comprises steps as follows: (1), phosphoric trichloride and alkyl primary amine react in the presence of the organic solvent and an acid-binding agent, and alkyl amino phosphorodichloridate is generated; (2), a reaction liquid in the step (1) directly reacts with the liquid ammonia, temperature returning is performed, and N-alkyl substituted phosphoric triamide is generated. The liquid ammonia is preferably added in the step (2), and a reaction liquid in the step (1) is added for a reaction. According to the production method, a procedure can be intermittent or continuous, an intermediate is not required to be purified, the reaction condition is mild, few byproducts are produced, the yield is good, the purity is high, and the production method is suitable for industrial production.
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Paragraph 0045; 0047
(2017/02/23)
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- A N-hydrocarbyl thiophosphoro phosphoric triamide method for the production of (by machine translation)
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This invention involves a kind of N-hydrocarbyl thiophosphoro phosphoric triamide method of production, comprising the following steps : (1) compound in the organic solvent and the presence of acid, trichloro with hydrocarbyl reaction of primary amine, acid, generating hydrocarbyl amidogen phosphinylidyne two chlorine ; (2) step (1) after filtration of a reaction liquid in the reaction with ammonia, generating N-hydrocarbyl thiophosphoro phosphoric triamide. Step (1) the preferred composite acid-binding agent and the mixture of the triethylamine. Said step (2) in the reaction process of participating in the reaction-hydrocarbyl N all phosphorothioic dichlorides N-hydrocarbyl of phosphorothioic dichlorides of the mass fraction of 1% - 10% of the returning. The production method of the invention can be intermittent or continuous, mild reaction conditions, there are few by-products, the yield is good, high purity, is easy to separate and purify, is suitable for industrial production. (by machine translation)
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Paragraph 0038; 0041
(2016/10/31)
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- PROCESS FOR PREPARING N-(HYDROCARBYL) PHOSPHORIC OR THIOPHOSPHORIC TRIAMIDES
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The invention provides a process for preparing N-(hydrocarbyl)phosphoric or thiophosphoric triamides with substantially improved yields and purity. Two equivalents of hydrocarbylamine are used in the reaction with phosphoryl or thiophosphoryl chloride and then with ammonia in an aromatic solvent. The invention further relates to N-(hydrocarbyl)phosphopric or thiophosphoric triamides having the purity of at least 98% wherein R is a hydrocarbyl group and X is O or S. [in-line-formulae](RNH)(NH2)2P=X ??(I)[/in-line-formulae]
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Page/Page column 3
(2011/08/22)
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- PROCESS FOR THE PREPARATION OF TRIAMIDES FROM AMMONIA AND AMIDODICHLORIDES
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The invention relates to a process for the preparation of triamides from ammonia and amido-dichlorides.
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Page/Page column 4
(2011/02/25)
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- A PROCESS FOR PREPARING N-(HYDROCARBYL) PHOSPHORIC OR THIOPHOSPHORIC TRIAMIDES
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The invention provides a process for preparing N-(hydrocarbyl)phosphoric or thiophosphoric triamides with substantially improved yields and purity. Two equivalents of hydrocarbylamine are used in the reaction with phosphoryl or thiophosphoryl chloride and then with ammonia in an aromatic solvent. The invention further relates to N-(hydrocarbyl)phosphopric or thiophosphoric triamides having the purity of at least 98 %.
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Page/Page column 11
(2010/05/13)
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- Method of Separating Acids from Chemical Reaction Mixtures by Means of Apolar Amines
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A process for the removal of acids from reaction mixtures, comprising at least one product of value which is sparingly soluble in water, by at least one unpolar amine as an auxiliary base, which includes: a) reacting the auxiliary base with the acid with formation of a salt; b) reacting the salt formed in step a) with a further base which accepts the acid with liberation of the auxiliary base and combines with the acid to be accepted from the auxiliary base to form a salt which is very readily soluble in water; c) extraction of the mixture obtained in step b) with water or an aqueous medium, wherein the salt of the further base dissolves in the aqueous phase and the product of value, or the solution of the product of value, in a suitable solvent and the auxiliary base form at least one separate nonaqueous phase; and d) removal by distillation of at least part of any solvent present from the at least one nonaqueous phase obtained in step c), to form two nonmiscible liquid phases.
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Page/Page column 7
(2008/12/09)
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