阅读说明：本技术 一种锂电池材料用氟化碳的制备方法 (A kind of preparation method of lithium battery material fluorocarbons ) 是由 谢子卓 谢学归 谢洁珊 张雨寒 于铉 于 2019-08-06 设计创作，主要内容包括：本发明提供了一种锂电池材料用氟化碳的制备方法,包括：步骤1、将碳源粉碎后,与铵盐,粘结剂混合后,加入工业乙醇,在50～100℃下加热；步骤2、烘干后转入反应釜内,通入氟气进行氟化生产。该制备方法在进行氟化生产之前先将碳源与铵盐,粘结剂混合后,加入工业乙醇,在50～100℃下加热烘干。用该法使得碳源内部的氟化反应完全,所生产的电池级氟化碳的克容量高达1010mAh/克,比未加任何处理的碳源生产的氟化碳克容量提高了26.25％,同时提高了安全性。(The present invention provides a kind of preparation methods of lithium battery material fluorocarbons, comprising: step 1 after crushing carbon source, is added industrial alcohol, heats at 50~100 DEG C with ammonium salt after binder mixing；It is transferred in reaction kettle after step 2, drying, is passed through fluorine gas and carries out fluorination production.Before carrying out fluorination production first industrial alcohol, the heating, drying at 50~100 DEG C is added after binder mixing in carbon source and ammonium salt by the preparation method.Make the fluorination reaction inside carbon source complete with the method, the gram volume of LITHIUM BATTERY fluorocarbons produced is up to 1010mAh/ grams, than not adding the fluorocarbons gram volume of carbon source production of any processing to improve 26.25%, while improving safety.)

1. a kind of preparation method of lithium battery material fluorocarbons, which is characterized in that described method includes following steps:

Step 1 after crushing carbon source, is added industrial alcohol, heats at 50~100 DEG C with ammonium salt after binder mixing；

It is transferred in reaction kettle after step 2, drying, is passed through fluorine gas and carries out fluorination production.

2. the preparation method of lithium battery material fluorocarbons as described in claim 1, which is characterized in that carbon in the step 1 Source includes petroleum coke, artificial graphite, at least one of natural graphite.

3. the preparation method of lithium battery material fluorocarbons as described in claim 1, which is characterized in that in the step 1, institute Stating ammonium salt includes any one in ammonium chloride or ammonium fluoride.

4. the preparation method of lithium battery material fluorocarbons as described in claim 1, which is characterized in that in the step 1, institute Stating binder includes any one in ptfe emulsion or inclined tetrafluoroethene lotion.

5. the preparation method of lithium battery material fluorocarbons as described in claim 1, which is characterized in that in the step 1, institute The weight ratio for stating carbon source and ammonium salt is 20~60:1；The carbon source and the weight ratio of binder are 10~30:1；The carbon source with The dosage weight ratio of industrial alcohol is 10~20:1.

6. the preparation method of lithium battery material fluorocarbons as described in claim 1, which is characterized in that in the step 1, institute The weight ratio for stating carbon source and ammonium salt is 40:1；The carbon source and the weight ratio of binder are 20:1；The carbon source and industrial alcohol Dosage weight ratio be 15:1.

7. the preparation method of lithium battery material fluorocarbons as described in claim 1, which is characterized in that add in the step 1 Hot temperature is 100 DEG C, and heating time is 1~3h.

8. the preparation method of lithium battery material fluorocarbons as described in claim 1, which is characterized in that fluorine in the step 2 It is 400~500 DEG C that metaplasia, which produces temperature,.

9. the preparation method of lithium battery material fluorocarbons as described in claim 1, which is characterized in that fluorine in the step 2 The specific steps that metaplasia produces are as follows: 400~500 DEG C are first warming up to, starting to be passed through pressure in pure fluorine gas to kettle is 1.8~2.2 kilograms, Start to react, pressure in kettle is emptied after 15~25min；Then proceed to be passed through fluorine gas to 1.8~2.2 kilograms of pressure, the reaction was continued, Pressure in kettle is emptied after 15~25min；So circulation, until end of reaction.

Technical field

The present invention relates to lithium battery material technical field more particularly to a kind of preparation sides of lithium battery material fluorocarbons Method.

Background technique

Lithium fluorocarbon battery is a kind of novel lithium primary battery.With voltage height, high-temperature behavior is outstanding, storage life It is long, it is safe and reliable the advantages that.The core material of lithium fluorocarbon battery is fluorocarbons, main using fluorine gas and carbon source are straight at high temperature It is prepared by the reversed mode answered.The pyroreaction of fluorine gas and carbon is very complicated, and the fluorine carbon ratio of fluorocarbons generated is widely different.At present The method that field uses has solidification bed process, when solidification bed process prepares fluorocarbons, since material is fixed, in carbon source surface and carbon source Portion's reaction is unbalanced, and fluorination effect is different.When surface is perfluorinated to be finished, the fluorination reaction inside carbon source is inadequate, fluorine Carbon ratio is lower, causes the gram volume of LITHIUM BATTERY fluorocarbons produced low, not higher than in 800mAh/ grams；If can continue to be fluorinated, The perfluorinated fluorocarbons finished in surface lacks the danger that may be exploded, and there are security risks.

Summary of the invention

The purpose of the present invention is to overcome the defects in the prior art, provides a kind of preparation of lithium battery material fluorocarbons The gram volume of method, LITHIUM BATTERY fluorocarbons produced is up to 1010mAh/ grams, with the carbon source production than not adding any processing Fluorocarbons gram volume (800mAh/ grams) improves 26.25%, and improves safety.

The present invention is implemented as follows:

The present invention provides a kind of preparation methods of lithium battery material fluorocarbons, and described method includes following steps:

Step 1 after crushing carbon source, is added industrial alcohol after binder mixing with ammonium salt, adds at 50~100 DEG C Heat；

It is transferred in reaction kettle after step 2, drying, is passed through fluorine gas and carries out fluorination production.

Preferably, carbon source includes petroleum coke, artificial graphite, at least one of natural graphite in the step 1.

Preferably, in the step 1, the ammonium salt includes any one in ammonium chloride or ammonium fluoride.It is further preferable that The ammonium salt is ammonium chloride.

Preferably, in the step 1, the binder includes times in ptfe emulsion or inclined tetrafluoroethene lotion It anticipates one kind.It is further preferable that the binder includes ptfe emulsion；The concentration of the ptfe emulsion is preferably 50%~70%；Most preferably, selecting concentration is 60% ptfe emulsion.The concentration of the inclined tetrafluoroethene lotion Preferably 100%.

Preferably, in the step 1, the weight ratio of the carbon source and ammonium salt is 20~60:1；The carbon source and binder Weight ratio be 10~30:1；The carbon source and the dosage weight ratio of industrial alcohol are 10~20:1.It is further preferable that the step In rapid 1, the weight ratio of the carbon source and ammonium salt is 40:1；The carbon source and the weight ratio of binder are 20:1；The carbon source with The dosage weight ratio of industrial alcohol is 15:1.

Preferably, heating temperature is 100 DEG C in the step 1, and heating time is 1~3h.

Preferably, the specific steps of production are fluorinated in the step 2 are as follows: be first warming up to 400~500 DEG C, start to be passed through pure Pressure is 1.8~2.2 kilograms in fluorine gas to kettle, starts to react, and pressure in kettle is emptied after 15~25mi n；It then proceedes to be passed through fluorine For gas to 1.8~2.2 kilograms of pressure, the reaction was continued, and pressure in kettle is emptied after 15~25mi n；So circulation, until end of reaction.

The invention has the advantages that:

The preparation method of a kind of lithium battery material fluorocarbons provided by the invention, first by carbon before carrying out fluorination production Industrial alcohol, the heating, drying at 50~100 DEG C is added after binder mixing in source and ammonium salt.With method LITHIUM BATTERY produced Fluorocarbons gram volume can be than not adding the fluorocarbons gram volume of the carbon source production of any processing to improve 26.25%.Its principle are as follows:

After carbon source mixes after crushing with four fluorine emulsions and alcohol, the demulsification due to alcohol to four fluorine emulsions, entire object Material can become fluffy.When drying heating at moderate temperatures, the interior ammonium chloride mixed can be decomposed further, so that wait react Carbon source becomes more loose porous, in this way in subsequent carbon source fluorination reaction, can guarantee that inside and outside reaction is equal to the greatest extent Even, fluorination effect is good.After being disposed, fluorocarbons reaction kettle is added in carbon source, it is intermittent logical under the conditions of 400~500 DEG C Enter fluorine gas and carry out fluorination reaction, so that the fluorination reaction inside carbon source is complete, the gram volume of LITHIUM BATTERY fluorocarbons produced is high Up to 1010mAh/ grams, and improve safety.

Detailed description of the invention

Fig. 1-4 is the electron microscope for the lithium battery material fluorocarbons that embodiment 1 is prepared；

Fig. 5-6 is the electron microscope for the lithium battery material fluorocarbons that embodiment 2 is prepared；

Fig. 7-8 is the electron microscope for the lithium battery material fluorocarbons that embodiment 3 is prepared；

Fig. 9-10 is the electron microscope for the lithium battery material fluorocarbons that embodiment 4 is prepared；

Figure 11-12 is the electron microscope for the lithium battery material fluorocarbons that embodiment 5 is prepared；

Figure 13-14 is the electron microscope for the lithium battery material fluorocarbons that embodiment 6 is prepared；

Figure 15 is the graphite differential thermal analysis curve for the lithium battery material fluorocarbons that embodiment 1 is prepared.

Specific embodiment

Below with reference to embodiment, the present invention is furture elucidated.These embodiments be interpreted as being merely to illustrate the present invention and It is not intended to limit the scope of the invention.After having read the content of the invention recorded, those skilled in the art can be with The present invention is made various changes or modifications, these equivalence changes and modification equally fall into model defined by claims of the present invention It encloses.