阅读说明：本技术 一种硫酰胺的合成工艺 (Synthesis process of sulfamide ) 是由 邵新华 何正江 王荣洲 徐保华 程永进 于 2020-06-02 设计创作，主要内容包括：一种硫酰胺的合成工艺,通过酰化、排氨、溶解分层水解、中和、蒸馏、溶解、抽滤、再蒸馏、结晶离心、精致后得到硫酰胺成品。本发明成本低、工艺合理,在合成过程中,产生的大部分废气可以通过冷凝装置回收利用,生产过程中产生的丙酮、甲醇、乙醇可以通过蒸馏回收再利用,极大地降低了生产成本。(A process for synthesizing sulfamide includes such steps as acylation, removing ammonia, dissolving, hydrolysis, neutralizing, distilling, dissolving, suction filtering, distilling again, crystallizing, centrifugal separation and refining. The invention has low cost and reasonable process, most of the generated waste gas can be recycled by a condensing device in the synthesis process, and the acetone, the methanol and the ethanol generated in the production process can be recycled by distillation, thereby greatly reducing the production cost.)

1. A synthesis process of sulfamide is characterized by comprising the following steps:

(1) pumping 50-60 parts of sulfuryl chloride into a 500L high-position kettle, and freezing and cooling the sulfuryl chloride at the temperature below-10 ℃ for later use;

(2) pumping 20-30 parts of n-octane into a 2000L self-priming synthesis kettle at room temperature, starting an ammonia self-control electromagnetic valve power supply when starting refrigeration and cooling to below-10 ℃, starting introducing 10-20 parts of ammonia into the kettle, starting a pressure release valve, and sampling; when the vapor pressure of ammonia and the vapor pressure of oxygen are more than 9:1, starting stirring, gradually increasing the stirring speed to 350R/min, controlling the temperature in the kettle to be below-10 ℃, starting to dropwise add sulfuryl chloride under the pressure of 0.08MPa, stopping introducing ammonia when the pressure continuously increases to 0.1MPa, maintaining for 15min, and determining that the reaction is finished when the pressure does not decrease;

(3) opening an emptying valve on a kettle, starting stirring, controlling the stirring to be below 200R/min, performing an ammonia discharging process, allowing ammonia gas to enter a falling film absorption tower for absorption, after ammonia discharging is finished, adding tap water, stirring to be completely dissolved, transferring to a layering kettle, standing for layering, returning an organic phase to an ammonification kettle for reuse, transferring an inorganic phase to a hydrolysis kettle, dropwise adding hydrochloric acid, adjusting the pH to be =3-4, heating for hydrolysis, after hydrolysis is finished for 1-2 hours, adjusting the pH to be neutral by using 20% ammonia water, performing reduced pressure distillation and dehydration to be dry, adding a methanol and ethanol mixed solution with water as necessary, adding acetone for reflux dissolution, performing suction filtration, selling solid ammonium salt as a byproduct, pumping a liquid phase to a 1000L crystallization kettle, evaporating two thirds of acetone, cooling and crystallizing, performing suction filtration, recovering and reusing a filtrate, transferring a crude sulfamide to a refining kettle, adding a metered methanol and ethanol mixed solution, and heating, adding weighed active carbon, carrying out suction filtration after 5-10 minutes, pumping filtrate to a 1000L crystallization kettle, cooling for crystallization, centrifuging to obtain a wet product of sulfamide, pumping centrifugal raffinate to a 1000L distillation kettle, and distilling to recover methanol and ethanol; putting wet sulfamide into a double-cone dryer, sealing the feeding hole, starting a double cone, starting a hot water pump, opening a steam valve of a hot water tank, heating and drying at the temperature of 40-50 ℃ for 3 hours; controlling the temperature at 50-65 ℃, drying for 14 hours, and controlling the drying weight loss to be less than or equal to 0.5%; and after drying is finished, closing a steam valve, changing cold water, cooling to below 40 ℃, discharging and packaging to obtain a sulfamide finished product.

2. The process according to claim 1, wherein the ratio of methanol to ethanol in the mixture of methanol and ethanol in step 3) is 1: 2.

3. The process according to claim 1, wherein the double cone vacuum in step 3) is not less than-0.07 MPa.

Technical Field

The invention relates to the technical field of chemical synthesis processes, in particular to a synthesis process of sulfamide.

Background

Sulfamide, also known as diaminosulfonyl, sulfamide. Formula SO2(NH2) 2. Molecular weight 96.11. The orthorhombic plate crystal can absorb dry ammonia gas at normal temperature to generate colorless ammonia complex, and has stable neutral property in acidic, neutral and alkaline aqueous solutions.

The sulfamide is synthesized by substituting sulfur by common amide and a corresponding sulfurization reagent, wherein the common sulfurization reagent is phosphorus pentasulfide and an aromatic hydrocarbon derivative Laweson reagent thereof: the Laweson reagent can also be used as an efficient vulcanizing reagent such as ketone, ester, enamine and the like, and the synthesis method comprises the steps of dissolving amide and the vulcanizing reagent in an organic solvent, and reacting for 10 hours at normal temperature under the protection of nitrogen. It was found experimentally that hydrogen sulfide and nitrile can also be examined to prepare thioamides under amine catalysis: the reaction mechanism is that amine and hydrogen sulfide form ammonium salt, the hydrogen sulfide negative ions in the ammonium salt attack carbon atoms of nitrile, meanwhile, the ammonium positive ions attack nitrogen atoms, and finally, hydrogen atoms of sulfydryl are subjected to intramolecular rearrangement to obtain sulfamide. The method has low preparation efficiency and high cost.

Disclosure of Invention

The invention aims to provide a synthesis process of sulfamide, which aims to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: a synthesis process of sulfamide comprises the following steps:

1) pumping 50-60 parts of sulfuryl chloride into a 500L high-position kettle, and freezing and cooling the sulfuryl chloride at the temperature below-10 ℃ for later use;

2) pumping 20-30 parts of n-octane into a 2000L self-priming synthesis kettle at room temperature, starting an ammonia self-control electromagnetic valve power supply when starting refrigeration and cooling to below-10 ℃, starting introducing 10-20 parts of ammonia into the kettle, starting a pressure release valve, and sampling; when the vapor pressure of ammonia and the vapor pressure of oxygen are more than 9:1, starting stirring, gradually increasing the stirring speed to 350R/min, controlling the temperature in the kettle to be below-10 ℃, starting to dropwise add sulfuryl chloride under the pressure of 0.08MPa, stopping introducing ammonia when the pressure continuously increases to 0.1MPa, maintaining for 15min, and determining that the reaction is finished when the pressure does not decrease;

3) opening an emptying valve on a kettle, starting stirring, controlling the stirring to be below 200R/min, performing an ammonia discharging process, allowing ammonia gas to enter a falling film absorption tower for absorption, after ammonia discharging is finished, adding tap water, stirring to be completely dissolved, transferring to a layering kettle, standing for layering, returning an organic phase to an ammonification kettle for reuse, transferring an inorganic phase to a hydrolysis kettle, dropwise adding hydrochloric acid, adjusting the pH to be =3-4, heating for hydrolysis, after hydrolysis is finished for 1-2 hours, adjusting the pH to be neutral by using 20% ammonia water, performing reduced pressure distillation and dehydration to be dry, adding a methanol and ethanol mixed solution with water as necessary, adding acetone for reflux dissolution, performing suction filtration, selling solid ammonium salt as a byproduct, pumping a liquid phase to a 1000L crystallization kettle, evaporating two thirds of acetone, cooling and crystallizing, performing suction filtration, recovering and reusing a filtrate, transferring a crude sulfamide to a refining kettle, adding a metered methanol and ethanol mixed solution, and heating, adding weighed active carbon, carrying out suction filtration after 5-10 minutes, pumping filtrate to a 1000L crystallization kettle, cooling for crystallization, centrifuging to obtain a wet product of sulfamide, pumping centrifugal raffinate to a 1000L distillation kettle, and distilling to recover methanol and ethanol; putting wet sulfamide into a double-cone dryer, sealing the feeding hole, starting a double cone, starting a hot water pump, opening a steam valve of a hot water tank, heating and drying at the temperature of 40-50 ℃ for 3 hours; controlling the temperature at 50-65 ℃, drying for 14 hours, and controlling the drying weight loss to be less than or equal to 0.5%; and after drying is finished, closing a steam valve, changing cold water, cooling to below 40 ℃, discharging and packaging to obtain a sulfamide finished product.

Preferably, the ratio of methanol to ethanol in the mixed solution of methanol and ethanol in the step 3) is 1: 2.

Preferably, the vacuum in the double cones in the step 3) is not lower than-0.07 MPa.

The invention has low cost and reasonable process, most of the generated waste gas can be recycled by a condensing device in the synthesis process, and the acetone, the methanol and the ethanol generated in the production process can be recycled by distillation, thereby greatly reducing the production cost.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.