阅读说明：本技术 一种低温合成二硫化碳的方法 (A kind of method of low temperature synthesis carbon disulfide ) 是由 梁初 潘良斌 曾称福 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：本发明公开了一种低温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,置于密闭的反应器中,通过低温加热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 kind of methods of low temperature synthesis carbon disulfide.The synthetic method is using lithium sulfide and carbon tetrachloride as raw material; under the protection of inert gas; lithium sulfide and carbon tetrachloride are mixed; it is placed in closed reactor; its reaction is set to generate carbon disulfide by the method for low-temperature heat; again by carrying out heating distillation separation solid and liquid to the product after reaction, by gained liquid, cooling solidifies carbon tetrachloride at a certain temperature, and liquid is carbon disulfide after separation of solid and liquid.The method of the present invention is easy to operate, and technique is convenient, and products therefrom is easily separated, and low energy consumption, and is easily industrialized production.)

1. a kind of method of low temperature synthesis carbon disulfide, which comprises the following steps:

(1) under the protection of inert gas, vulcanization lithium powder is uniformly mixed with carbon tetrachloride, is placed on closed reactor In；

(2) it reacts under the conditions of low-temperature heat and generates carbon disulfide；

(3) after reacting end and cooling down, the mixture after reaction is separated by solid-liquid separation by distillation mode；

(4) gained product liquid after distillation is cooled down at a certain temperature, solidifies carbon tetrachloride, gained liquid after separation of solid and liquid As carbon disulfide.

2. a kind of method of low temperature synthesis carbon disulfide as described in claim 1, which is characterized in that lazy described in step (1) Property gas is the gas not reacted with reactant and product or the mixture of gas, including nitrogen and argon gas.

3. a kind of method of low temperature synthesis carbon disulfide as described in claim 1, which is characterized in that sulphur described in step (1) The mass ratio of the material for changing lithium and carbon tetrachloride is 2:(1~3).

4. a kind of method of low temperature synthesis carbon disulfide as described in claim 1, which is characterized in that low described in step (2) Warm heating condition are as follows: be heated to 50~75 DEG C from room temperature by the heating speed of 1~20 DEG C/min, 1~100h of isothermal reaction.

5. a kind of method of low temperature synthesis carbon disulfide as described in claim 1, which is characterized in that divide described in step (3) It need to be carried out under the protection of inert gas from process, vapo(u)rizing temperature is 40~100 DEG C.

6. a kind of method of low temperature synthesis carbon disulfide as described in claim 1, which is characterized in that cold described in step (4) But temperature is -35~-25 DEG C.

Technical field

The invention belongs to technical field of chemical synthesis, a kind of method for relating generally to low temperature synthesis carbon disulfide.

Background technique

Carbon disulfide is a kind of important Inorganic Chemicals, widely used, is presently mainly used as solvent and as one The raw material of a little fine chemical product synthesis.As industrial chemicals, it to be used for synthesizing dimethyl thioether, dimethyl sulfoxide, dimethyl sulfone, Rubber vulcanization accelerator M, D, xanthates mineral flotation agent etc., it is also possible to make the vulcanizing agent of como shift catalyst etc.；As Solvent is mainly used for viscose rayon, the synthesis of glassine paper and insoluble sulfuy, grease, wax, resin, rubber production；Curing Carbon may further be used to manufacture pesticide, be used as insecticide and cereal fumigant.Currently, the raw material route of production carbon disulfide mainly has wood Charcoal -- sulfur method, coke -- sulfur method, natural gas -- sulfur method etc..

Most domestic manufacturer is using the production for producing carbon disulfide using sulphur and natural gas as raw material at present Method, this method have the characteristics of working condition is good, labor productivity is high, occupation area of equipment is small, high degree of automation, but due to It is to produce carbon disulfide using tubular type heating using natural gas and sulphur as raw material, i.e., in 600~800 DEG C of high temperature, high pressure 1.0 Gas phase reaction is carried out after sulphur gasifies under the conditions of~2.1Mpa in pipe, therefore natural gas act has the disadvantages that consumption of raw materials Amount is big；Every 1 ton of carbon disulfide of production generates about 900 kilograms of hydrogen sulfide gas simultaneously；A large amount of day is burnt while reaction Right gas；The investment cost of vent gas treatment is big after the recycling and recycling of hydrogen sulfide gas, equipment material require it is high.In addition, burnt Charcoal method for raw material, has energy consumption height, large labor intensity, single device production efficiency with sulphur and coke (past uses charcoal) Low, the shortcomings that equipment life is short and environmental pollution is serious, belongs to the production line that will be eliminated, but domestic at present still has 55% Manufacturer use the technique.

In addition, patent (application publication number CN101516775A) discloses a kind of method for preparing carbon disulfide, with an oxygen Change carbon and hydrogen sulfide is that raw material reaction generates carbonyl sulfide and hydrogen, carbonyl sulfide and catalyst haptoreaction is made to generate carbon dioxide and two Nitric sulfid.Pressure needed for preparing the method for carbon disulfide in the technical solution is higher, and temperature is higher, reaction raw materials H₂S and CO, energy consumption is high, higher cost, and has very big toxicity, will cause certain harm to environment and human body.Here, proposing one kind Easy to operate, technique is convenient, and product purity is high, and low energy consumption, it is easy to accomplish the carbon disulfide synthetic method of industrialized production.

Summary of the invention

It is an object of the present invention to solve the deficiency of the existing technology and provide a kind of equipment simply, operation is convenient, efficient, The method of low energy consumption is used to prepare and purifies carbon disulfide.

The method of low temperature synthesis carbon disulfide of the present invention, is to pass through low temperature using lithium sulfide and carbon tetrachloride as raw material The method of heating prepares carbon disulfide, and obtains the higher carbon disulfide of purity by the way of distillation.

The specific technical solution that the present invention solves the use of its technical problem is as follows:

The method of low temperature synthesis carbon disulfide of the present invention, comprising the following steps:

(1) under the protection of inert gas, dry vulcanization lithium powder is uniformly mixed with carbon tetrachloride, is placed on closed Reactor in；

(2) it reacts under the conditions of low-temperature heat and generates carbon disulfide；

(3) after reacting end and cooling down, the mixture after reaction is separated by solid-liquid separation by distillation mode；

(4) gained product liquid after distillation is cooled down at a certain temperature, solidifies carbon tetrachloride, gained after separation of solid and liquid Liquid is carbon disulfide.

Preferably, inert gas described in step (1) is the gas or gas not reacted with reactant and product The mixture of body, including nitrogen and argon gas.

Preferably, the mass ratio of the material of lithium sulfide described in step (1) and carbon tetrachloride is 2:(1~3).

Preferably, low-temperature heat condition described in step (2) are as follows: add by the heating speed of 1~20 DEG C/min from room temperature Heat is to 50~75 DEG C, 1~100h of isothermal reaction.

Preferably, separation process described in step (3) need to carry out under the protection of inert gas, vapo(u)rizing temperature be 40~ 100℃。

Preferably, cooling temperature described in step (4) is -35~-25 DEG C.

Compared with prior art, the present invention its advantages are mainly reflected in:

(1) low temperature synthesis carbon disulfide method equipment of the present invention is simple, and simple process, product is easily separated, and low energy consumption, is easy to Industrialized production.

(2) low temperature synthesis carbon disulfide method of the present invention carries out solid-liquid using lithium sulfide solid and carbon tetrachloride liquid as raw material Reaction can greatly improve yield with the advantage come into full contact between reactant.

Detailed description of the invention

Fig. 1 is the XRD diagram of the solid product after embodiment 1 is reacted after distillation separation, since product carbon disulfide is liquid Body has separated during the separation process, therefore remaining solid product.

Specific embodiment

With reference to the accompanying drawing, with specific embodiment, technical scheme is described further, but guarantor of the invention It is without being limited thereto to protect range.