阅读说明：本技术 一种合成黑色硫化汞的方法 (A kind of method of synthesizing black mercuric sulphide ) 是由 梁初 潘良斌 王凯 张文魁 甘永平 夏阳 张俊 黄辉 于 2019-08-26 设计创作，主要内容包括：本发明公开了一种合成黑色硫化汞的方法,所述的方法以氯化汞为汞源,硫化锂为硫源,均匀分散后,通过加热的方法使其反应生成硫化汞。待反应完成后,用去离子水或有机溶剂洗涤干净,在烘箱中烘干即得到纯的硫化汞。本发明方法,工艺简单,能耗低,易于工业化生产。(The invention discloses a kind of method of synthesizing black mercuric sulphide, for the method using mercury chloride as mercury source, lithium sulfide is sulphur source, after evenly dispersed, so that its reaction is generated mercuric sulphide by the method for heating.It is clean with deionized water or organic solvent washing to after the reaction was completed, it is obtained by drying in an oven to arrive pure mercuric sulphide.The method of the present invention, simple process, low energy consumption, easy to industrialized production.)

1. a kind of method of synthesizing black mercuric sulphide, which comprises the following steps:

(1) under vacuum or protective atmosphere, anhydrous mercury chloride and lithium sulfide are uniformly mixed, are transferred to closed reactor；

(2) mixture in reactor is heated to 100-300 DEG C, isothermal reaction 0.1-100h；

(3) after reaction, mercuric sulphide can be obtained in the solid product separation taken out in reactor.

2. a kind of method of synthesizing black mercuric sulphide as described in claim 1, it is characterised in that: guarantor described in step (1) Protecting atmosphere is the gas or their mixture not reacted with reactant and product, including nitrogen and argon gas.

3. a kind of method of synthesizing black mercuric sulphide as described in claim 1, it is characterised in that: nothing described in step (1) The molar ratio of water mercury chloride and lithium sulfide is 1:1~3.

4. a kind of method of synthesizing black mercuric sulphide as described in claim 1, it is characterised in that: heating process in step (2) Heating rate is 0.5 DEG C/min-20 DEG C/min.

5. a kind of method of synthesizing black mercuric sulphide as described in claim 1, it is characterised in that: separation described in step (3) It is to be dissolved in solid product in deionized water or organic solvent, is filtered, washed, 80-85 DEG C of baking oven drying, organic solvent packet Include ethyl alcohol or acetone.

Technical field

The invention belongs to the preparation technical fields of function nano material, relate generally to a kind of side of synthesizing black mercuric sulphide Method.

Background technique

The precipitating of the mercuric sulphide Environmental Chemistry process basic as one with dissolution, to environment shape of the mercury in surrounding medium State distribution, migration, reactivity and corresponding Transport And Transformation play key effect, and the critical process of control Hg toxicity.By In some difficulties in the toxicity and preparation of mercury, the chalcogenide materials research in relation to mercury is fewer.Usually prepare black sulphur Change the method for mercury mainly by the way that hydrogen sulfide gas to be passed through in mercury salt solution, this method is easy to happen the leakage of gas, pollutes ring Border.Mercury and sulphur powder are mainly heated to 140 DEG C~160 DEG C generation frit reactions by the method for preparation of industrialization mercuric sulphide, due to being Exothermic reaction, sulphur powder are easy to happen spontaneous combustion, and production hidden danger is bigger.

Mercuric sulphide due to having higher electron mobility, low forbidden bandwidth and significant thermoelectricity and infrared ray optical direction effect, To show broad application prospect in terms of infrared device material.

Chinese invention patent (104591262 A of application publication number CN), which discloses a kind of dropwise addition reflux and prepares mercuric sulphide, to be received The method of rice corpuscles takes mercury source raw material to be configured to mercury source aqueous solution, thioacetamide is taken to be configured to aqueous solution, and a kind of solution is turned It moves on in three-neck flask, another solution is added in flask while stirring, and reacting under magnetic agitation heating device can prepare At mercuric sulphide.Chinese invention patent (109437281 A of application publication number CN) discloses a kind of chiral metal compound nanometer material The aqueous phase preparation method for expecting mercuric sulphide, using mercury salt aqueous solution and sulfide solution as reaction raw materials, sulfur-containing amino acid is chirality Inducer is reacted in 20-50 DEG C of stirred in water bath, the chiral metal compound nano material vulcanization of final obtained size uniformity Mercury.Although when preparing mercuric sulphide material, nearly all being used currently, can obtain the mercuric sulphide with specific structure It is unfavorable for the organic solvent of environmental ecology or the hydro-thermal method of chemical industry surfactant and high energy consumption.Therefore develop it is environmentally protective, The method of the synthesis mercuric sulphide material of simple process still has challenge.

Summary of the invention

In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of simple, environmentally protective, low energy consumption synthesis is black The method of color mercuric sulphide.

The present invention is respectively mercury source and sulphur source using anhydrous mercury chloride and lithium sulfide, makes its hair by the method for low-temperature heat Raw reaction synthesis mercuric sulphide.

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

A kind of method of synthesizing black mercuric sulphide, steps are as follows:

(1) under vacuum or protective atmosphere, anhydrous mercury chloride and lithium sulfide are fitted into closed reactor, are heated to 100-300 DEG C, constant temperature reacts 0.1-100h；

(2) after reaction, mercuric sulphide is can be obtained into the solid product separation of taking-up.

Preferably, protective atmosphere described in step (1) be the gas not reacted with reactant and product or it Mixture, including nitrogen and argon gas.

Preferably, the molar ratio of anhydrous mercury chloride described in step (1) and lithium sulfide is 1:1~3.

Preferably, the heating rate of heating process is 0.5 DEG C/min-20 DEG C/min in step (1).

Preferably, separation method described in step (2) is that solid product is dissolved in deionized water or organic solvent, filtering Drying is washed, organic solvent includes ethyl alcohol or acetone.

Compared with prior art, the present invention its advantages are mainly reflected in: the method for the present invention simple process, it can be in low temperature Lower reaction, low energy consumption, easy to industrialized production, and by-product unharmful substance is environmentally protective.

Detailed description of the invention

Fig. 1 is the XRD diagram that dry mercuric sulphide is washed after embodiment 1 is reacted.

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.