阅读说明：本技术 超细无定形硼粉的制备方法 (Preparation method of superfine amorphous boron powder ) 是由 喇培清 董晨晨 朱敏 郑月红 占发琦 石玉 毛宇奇 刘海斌 王娇 安宁 于 2020-07-02 设计创作，主要内容包括：本发明属于硼粉制备技术领域。为了获得高纯度、低粒径的超细无定形硼粉,本发明公开了一种超细无定形硼粉的制备方法。该超细无定形硼粉的制备方法,具体包括以下步骤：步骤S1,秤取反应原料；按质量百分比计,反应原料包括Mg粉末40～48％、B<Sub>2</Sub>O<Sub>3</Sub>粉末35～42％、稀释剂粉末10～24％；步骤S2,对反应原料进行混合处理,并对混合后的反应原料进行加压处理,获得圆饼状坯体；步骤S3,进行镁热反应,制备获得含有硼粉的块状物。步骤S4,采用酸洗-水洗的浸洗工艺,对获得含有硼粉的块状物进行杂质去除,得到高纯度、低粒径的超细无定形硼粉。采用本发明的方法不仅可以高纯度、低粒径的超细无定形硼粉,而且可以降低制造成本,提高生产效率。(The invention belongs to the technical field of boron powder preparation. The invention discloses a preparation method of superfine amorphous boron powder in order to obtain the superfine amorphous boron powder with high purity and low particle size. The preparation method of the superfine amorphous boron powder specifically comprises the following steps: step S1, weighing reaction raw materials; according to mass percentage, the reaction raw materials comprise 40-48% of Mg powder and B 2 O 3 35-42% of powder and 10-24% of diluent powder; step S2, mixing the reaction raw materials, and pressurizing the mixed reaction raw materials to obtain a round cake-shaped blank; and step S3, performing magnesium thermal reaction to prepare and obtain a block containing boron powder. And step S4, removing impurities from the obtained block containing the boron powder by adopting an acid washing-water washing immersion washing process to obtain the superfine amorphous boron powder with high purity and low particle size. The method of the invention not only can be used for preparing the superfine amorphous boron powder with high purity and low particle size, but also can reduce the manufacturing cost and improve the production efficiency.)

1. The preparation method of the superfine amorphous boron powder is characterized by comprising the following steps:

step S1, weighing reaction raw materials; according to mass percentage, the reaction raw materials comprise 40-48% of Mg powder and B₂O₃35-42% of powder and 10-24% of diluent powder, wherein the diluent powder is KCl or MgCl₂And NaCl;

step S2, mixing the reaction raw materials, and pressurizing the mixed reaction raw materials to obtain a round cake-shaped blank;

step S3, firstly, placing the blank into a combustion synthesis reaction kettle, and placing an ignition agent on the upper surface of the blank; secondly, filling 0.5MPa of argon into the reaction kettle, discharging the gas in the reaction kettle to 0 when the temperature in the reaction kettle is heated to 110-130 ℃, stopping gas discharge, completely discharging the gas in the reaction kettle when the temperature in the reaction kettle is heated to 170-190 ℃ again, and preserving the temperature for 0.5 h; then filling argon into the reaction kettle again to increase the pressure in the reaction kettle to 1-3 Mpa; when the temperature in the reaction kettle rises to 250-270 ℃, magnesium thermal reaction is carried out in the reaction kettle; and finally, after the magnesium thermal reaction is finished and the temperature is cooled to the room temperature, obtaining the block containing the boron powder.

And step S4, removing impurities from the obtained block containing the boron powder by adopting an acid washing-water washing immersion washing process to obtain the superfine amorphous boron powder with high purity and low particle size.

2. The method for preparing ultra-fine amorphous boron powder as claimed in claim 1, wherein in the step S1, the reaction raw materials comprise 43-47% by mass of Mg powder and B₂O₃37-40% of powder and 13-20% of KCl powder.

3. The method for preparing ultra-fine amorphous boron powder as claimed in claim 1, wherein in the step S1, the reaction raw materials comprise 40-45% by mass of Mg powder and B₂O₃35-40% of powder and MgCl₂16-24% of powder.

4. The ultra-fine amorphous boron powder of claim 1The preparation method of (1) is characterized in that in the step S1, the reaction raw materials comprise 44-48% by mass of Mg powder and B₂O₃38-42% of powder and 10-16% of NaCl powder.

5. The method for producing an ultrafine amorphous boron powder as defined in claim 1, wherein in said step 4, first, the cake containing boron powder obtained by the reaction is pulverized by a pulverizer to obtain a powder containing boron powder; then, adopting 12mol/L hydrochloric acid as a pickling agent to carry out pickling treatment; then, washing the acid-washed product until the acid-washed product is neutral, and centrifuging the acid-washed product by using a centrifugal machine to obtain a target product; and finally, drying the centrifuged target product in a vacuum drying oven at 100 ℃ for 12h to obtain the final high-purity low-particle-size superfine amorphous boron powder.

6. The method for preparing an ultrafine amorphous boron powder according to claim 5, wherein, in the pickling process, the solution after pickling is detected by a pH indicator to determine whether pickling is complete; wherein if the pH indicator shows neutral or alkaline, continuing to add the lotion; if the pH indicator shows acidity, the addition of the lotion is stopped.

7. The method for preparing ultra fine amorphous boron powder as claimed in claim 5, wherein the pickling process is performed in an enamel reactor with the stirrer kept on.

8. The method for preparing an ultra-fine amorphous boron powder as claimed in claim 1, wherein in the step S2, the reaction raw material is green-pressed using a pressure of 15MPa to 45 MPa.

Technical Field

The invention belongs to the technical field of boron powder preparation, and particularly relates to a preparation method of superfine amorphous boron powder.

Background

The amorphous boron powder has the advantages of large specific surface area, high combustion heat value, convenient carrying and the like, has wide application, is mainly used for synthesizing new metallurgical materials and boron-rich fuels in the fields of aviation, aerospace and military and also can be used as an initiator of an air bag.

Currently, methods for preparing amorphous boron powder include molten salt electrolysis, diborane cracking, borohydride halide reduction, metallothermic reduction, and the like. Among them, molten salt electrolysis cannot be further developed and popularized due to the limitations of low current efficiency, severe working environment and discontinuous production. Although high-purity boron powder can be obtained by diborane cracking and borohydride halide reduction, the large-range popularization and application of the method are restricted by the high-requirement operating environment and serious pollution. The Boron powder with the Boron content of 92.43% can be prepared by a self-propagating metallurgy method, but the average particle size of the Boron powder does not meet the requirement of the American SB Boron95 on the Boron powder, and the SBboron95 requires that the average particle size of the Boron powder is 0.8-1.0 μm.

Disclosure of Invention

The invention provides a preparation method of superfine amorphous boron powder, aiming at obtaining the superfine amorphous boron powder with high purity and low particle size. The preparation method of the superfine amorphous boron powder specifically comprises the following steps:

step S1, weighing reaction raw materials; according to mass percentage, the reaction raw materials comprise 40-48% of Mg powder and B₂O₃35-42% of powder and 10-24% of diluent powder, wherein the diluent powder is selected fromKCl、MgCl₂And NaCl;

step S2, mixing the reaction raw materials, and pressurizing the mixed reaction raw materials to obtain a round cake-shaped blank;

step S3, firstly, placing the blank into a combustion synthesis reaction kettle, and placing an ignition agent on the upper surface of the blank; secondly, filling 0.5MPa of argon into the reaction kettle, discharging the gas in the reaction kettle to 0 when the temperature in the reaction kettle is heated to 110-130 ℃, stopping gas discharge, completely discharging the gas in the reaction kettle when the temperature in the reaction kettle is heated to 170-190 ℃ again, and preserving the temperature for 0.5 h; then filling argon into the reaction kettle again to increase the pressure in the reaction kettle to 1-3 Mpa; when the temperature in the reaction kettle rises to 250-270 ℃, magnesium thermal reaction is carried out in the reaction kettle; and finally, after the magnesium thermal reaction is finished and the temperature is cooled to the room temperature, obtaining the block containing the boron powder.

And step S4, removing impurities from the obtained block containing the boron powder by adopting an acid washing-water washing immersion washing process to obtain the superfine amorphous boron powder with high purity and low particle size.

Preferably, in the step S1, the reaction raw materials include, by mass, 43-47% of Mg powder and B₂O₃37-40% of powder and 13-20% of KCl powder.

Preferably, in the step S1, the reaction raw materials include, by mass, 40-45% of Mg powder and B₂O₃35-40% of powder and 16-24% of MgCl2 powder.

Preferably, in the step S1, the reaction raw materials include, by mass, 44-48% of Mg powder and B₂O₃38-42% of powder and 10-16% of NaCl powder.

Preferably, in the step 4, firstly, the lump containing the boron powder obtained by the reaction is pulverized by a pulverizer to obtain a powder containing the boron powder; then, adopting 12mol/L hydrochloric acid as a pickling agent to carry out pickling treatment; then, washing the acid-washed product until the acid-washed product is neutral, and centrifuging the acid-washed product by using a centrifugal machine to obtain a target product; and finally, drying the centrifuged target product in a vacuum drying oven at 100 ℃ for 12h to obtain the final high-purity low-particle-size superfine amorphous boron powder.

Preferably, in the pickling treatment process, a pH indicator is used for detecting the solution after pickling to judge whether pickling is complete; wherein if the pH indicator shows neutral or alkaline, continuing to add the lotion; if the pH indicator shows acidity, the addition of the lotion is stopped.

It is further preferred that during the pickling process, the work is carried out in an enamel reactor and the stirrer is continuously switched on.

Preferably, in the step S2, the reaction raw material is green-pressed by using a pressure of 15MPa to 45 MPa.

The invention has the following beneficial effects:

1. according to the method, the mixed powder is composed of the magnesium powder, the diboron trioxide powder and the diluent powder which are low in cost, the boron powder-containing block is prepared by adopting the magnesium thermal reaction with low cost and low energy consumption, and the high-purity low-particle-size superfine amorphous boron powder can be obtained after the boron powder-containing block is subjected to acid washing, water washing, centrifugation and drying in sequence. Therefore, the method not only achieves the aim of preparing amorphous boron powder with low cost and low energy consumption, reduces the cost for preparing superfine amorphous boron powder, improves the efficiency for preparing superfine amorphous boron powder, but also obtains the superfine amorphous boron powder with high purity and low particle size, and meets the popularization and application in the fields of new metallurgical materials, aviation, aerospace and military.

2. In the process of the present invention, the diluent powder may be KCl or MgCl, depending on the case₂And NaCl, and selecting the type of the diluent according to the difference, and matching the Mg powder and the B powder in corresponding mass percentage₂O₃The powder can ensure that the superfine amorphous boron powder is finally obtained, thereby realizing the effect of preparing the superfine amorphous boron powder by different mixed components, meeting the requirements of low-cost and high-efficiency preparation of the superfine amorphous boron powder by adopting the method under different working conditions, and improving the efficiency of the preparation method of the amorphous boron powder.

Drawings

FIG. 1 is a schematic flow chart of the process for preparing a high purity, low particle size ultra-fine amorphous boron powder of example 1.

Detailed Description

The technical solution of the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.