阅读说明：本技术 一种机械球磨合成二硫化碳的方法 (Method for synthesizing carbon disulfide by mechanical ball milling ) 是由 梁初 曾称福 陈云 甘永平 夏阳 张俊 黄辉 张文魁 于 2019-08-26 设计创作，主要内容包括：本发明公开了一种机械球磨合成二硫化碳的方法。所述合成方法以硫化锂和四氯化碳为原料,在惰性气体的保护下,将硫化锂和四氯化碳混合,置于密闭的球墨罐中,在室温下,通过机械球磨的方法使其反应生成二硫化碳,再通过对反应后的产物进行加热蒸馏分离固体和液体,将所得液体在一定温度下冷却使四氯化碳凝固,固液分离后液体即为二硫化碳。本发明方法操作简单,工艺便捷,所得产物易分离,能耗低,且易于实现工业化生产。(The invention discloses a method for synthesizing carbon disulfide by mechanical ball milling. The synthesis method comprises the steps of taking lithium sulfide and carbon tetrachloride as raw materials, mixing the lithium sulfide and the carbon tetrachloride under the protection of inert gas, placing the mixture in a closed nodular graphite tank, reacting the mixture to generate carbon disulfide at room temperature by a mechanical ball milling method, heating and distilling a reaction product to separate solid and liquid, cooling the obtained liquid at a certain temperature to solidify the carbon tetrachloride, and separating the solid from the liquid to obtain the carbon disulfide. The method has the advantages of simple operation, convenient process, easy separation of the obtained product, low energy consumption and easy realization of industrial production.)

1. A method for synthesizing carbon disulfide by mechanical ball milling is characterized by comprising the following steps:

(1) Under the protection of inert gas, uniformly mixing lithium sulfide powder with carbon tetrachloride, and placing the mixture in a closed nodular graphite tank;

(2) carrying out mechanical ball milling reaction at room temperature to generate carbon disulfide;

(3) After the reaction is finished and cooled, carrying out solid-liquid separation on the reacted mixture in a distillation mode;

(4) And cooling the liquid product obtained after distillation at a certain temperature to solidify carbon tetrachloride, and performing solid-liquid separation to obtain liquid, namely carbon disulfide.

2. The method for synthesizing carbon disulfide by mechanical ball milling as claimed in claim 1, wherein the inert gas in step (1) is a gas or a mixture of gases which do not react with the reactants and products, and includes nitrogen and argon.

3. The method for synthesizing carbon disulfide by mechanical ball milling according to claim 1, wherein the mass ratio of lithium sulfide to carbon tetrachloride in step (1) is 2: (1-3).

4. The method for synthesizing carbon disulfide by mechanical ball milling according to claim 1, wherein the ratio of the total mass of the mixture of lithium sulfide and carbon tetrachloride to the total mass of the grinding balls in the step (2) is 1 (20-100).

5. The method for synthesizing carbon disulfide by mechanical ball milling according to claim 1, wherein the conditions of the mechanical ball milling reaction in the step (2) are as follows: the ball milling speed is 200-500 r/min, and the ball milling time is 2-100 h.

6. The method for synthesizing carbon disulfide by mechanical ball milling according to claim 1, wherein the separation process in the step (3) is carried out under the protection of inert gas, and the distillation temperature is 40-100 ℃.

7. The method for synthesizing carbon disulfide by mechanical ball milling according to claim 1, wherein the cooling temperature in the step (4) is-35 to-25 ℃.

Technical Field

the invention belongs to the field of chemical synthesis, and mainly relates to a method for synthesizing carbon disulfide by mechanical ball milling.

Background

Carbon disulfide is used as an important chemical raw material, is mainly used as a raw material for manufacturing viscose fiber and cellophane, and is used as a raw material for producing rayon, cellophane, pesticide bactericide and rubber auxiliary agent; carbon disulfide is an excellent solvent in the production of products such as grease, wax, resin, rubber, sulfur and the like; in addition, the composite can also be used as a mold release agent of paint and varnish, a clothes detergent, a metal flotation agent, an aviation kerosene additive, a wool degreasing agent and the like. At present, the method for preparing carbon disulfide mainly comprises two methods, namely a natural gas method (methane method) and a coke method (semi-coke method), the first method is a mainstream technology at present internationally and domestically, is a continuous production process, has small occupied area, large production scale and high automation degree, but because the carbon disulfide is produced by taking natural gas and sulfur as raw materials and adopting a tubular heating method, namely sulfur is gasified under the conditions that the reaction temperature is as high as 600-800 ℃ and the pressure is 1.0-2.1 Mpa and then gas-phase reaction is carried out in a tube, the method has the defects of large one-time investment, high production cost, reaction at high temperature and high pressure, safety problem, large production amount of side reactant hydrogen sulfide, reduction through a Rokes reduction reaction, large energy consumption and the like. In addition, only a few areas have conditional use of natural gas at present, so that the method is difficult to be applied on a large scale due to the influence of natural gas sources and other factors. The second coke method uses sulfur and coke (charcoal is used in the past) as raw materials, has the defects of high energy consumption, high labor intensity, low production efficiency of single equipment, short service life of the equipment, serious environmental pollution and the like, belongs to a production route to be eliminated, but 55 percent of manufacturers in China still adopt the process at present.

In addition, a patent (application publication No. CN101516775A) discloses a method for preparing carbon disulfide, in which carbon monoxide and hydrogen sulfide are used as raw materials to react to form carbonyl sulfide and hydrogen, and the carbonyl sulfide is contacted with a catalyst to react to form carbon dioxide and carbon disulfide. The method for preparing the carbon disulfide in the technical scheme has the advantages of higher required pressure and higher temperature, and the reaction raw material is H₂S and CO, high energy consumption, high cost, great toxicity and environment friendshipand human body may cause certain harm. The carbon disulfide synthesis method is simple to operate, convenient and fast in process, high in product purity, low in energy consumption and easy to realize industrial production.

Disclosure of Invention

The invention aims to overcome the defects in the prior art and provides a method which is simple in equipment, convenient and fast to operate, high in efficiency and low in energy consumption and is used for preparing and purifying carbon disulfide.

The method for synthesizing the carbon disulfide by mechanical ball milling provided by the invention is used for preparing the carbon disulfide by taking lithium sulfide and carbon tetrachloride as raw materials through the mechanical ball milling method, and the carbon disulfide with higher purity is obtained by adopting a distillation mode.

the invention adopts the following specific technical scheme for solving the technical problems:

The method for synthesizing the carbon disulfide by mechanical ball milling comprises the following steps:

(1) Under the protection of inert gas, uniformly mixing lithium sulfide powder with carbon tetrachloride, and placing the mixture in a closed nodular graphite tank;

(2) Carrying out mechanical ball milling reaction at room temperature to generate carbon disulfide;

(3) After the reaction is finished and cooled, carrying out solid-liquid separation on the reacted mixture in a distillation mode;

(4) And cooling the liquid product obtained after distillation at a certain temperature to solidify carbon tetrachloride, and performing solid-liquid separation to obtain liquid, namely carbon disulfide.

Preferably, the inert gas in step (1) is a gas or a mixture of gases that does not react with the reactants and products, and includes nitrogen and argon.

Preferably, the lithium sulfide and carbon tetrachloride in the step (1) are mixed according to the mass ratio of 2: (1-3) mixing.

preferably, the mechanical ball milling reaction conditions in the step (2) are as follows: the ratio of the total mass of the mixture of lithium sulfide and carbon tetrachloride to the total mass of the grinding balls is 1 (20-100), the ball milling rotating speed is 200-500 r/min, and the ball milling time is 2-100 h.

Preferably, the separation process in the step (3) needs to be carried out under the protection of inert gas, and the distillation temperature is 40-100 ℃.

Preferably, the cooling temperature in the step (4) is-35 to-25 ℃.

Compared with the prior art, the invention has the following beneficial effects:

(1) The method for synthesizing the carbon disulfide by mechanical ball milling has the advantages of simple equipment, simple and convenient process, high product purity, low energy consumption and easy industrial production.

(2) The method for synthesizing the carbon disulfide by the mechanical ball milling takes the lithium sulfide solid and the carbon tetrachloride liquid as raw materials to carry out solid-liquid reaction, has the advantage of full contact between reactants, and can greatly improve the yield.

Drawings

figure 1 is the XRD pattern of the solid product after the reaction of example 1 and after separation by distillation, since the product carbon disulfide, which is a liquid, has been separated during the separation, thus leaving a solid product.

Detailed Description

the technical solution of the present invention is further described with reference to the following embodiments, but the scope of the present invention is not limited thereto.