阅读说明：本技术 一种从水性钻石液中提取钻石粉的方法 (Method for extracting diamond powder from aqueous diamond liquid ) 是由 周群飞 罗彬彬 于 2018-07-10 设计创作，主要内容包括：本发明提供了一种从水性钻石废液中提取钻石粉的方法,包括以下步骤：A)过滤水性钻石抛光液,去除抛光液中的牙板碎渣；B)加入浓盐酸,搅拌后静置分液,进行抽滤,得到钻石粉富集液；所述浓盐酸的质量分数为20～25％；C)将钻石粉富集液进行去离子水清洗,然后加入氢氧化钠溶液,进行碱化反应；D)将所述碱化反应后的钻石粉富集液进行去离子水清洗,然后进行烘干,得到钻石粉。本发明中的方法能够将废液进行资源回收利用,同时也能将废液集中处理,从而节约了资源,降低了生产成本,可大大减少辅料的浪费。实验结果证明,本申请中的方法钻石粉的回收率为81～85％。(The invention provides a method for extracting diamond powder from aqueous diamond waste liquid, which comprises the following steps: A) filtering the aqueous diamond polishing solution, and removing dental plate debris in the polishing solution; B) adding concentrated hydrochloric acid, stirring, standing for liquid separation, and performing suction filtration to obtain a diamond powder enrichment solution; the mass fraction of the concentrated hydrochloric acid is 20-25%; C) washing the diamond powder enrichment solution with deionized water, and then adding a sodium hydroxide solution for an alkalization reaction; D) and washing the diamond powder enriched solution after the alkalization reaction by using deionized water, and then drying to obtain the diamond powder. The method can recycle the resources of the waste liquid and simultaneously can treat the waste liquid in a centralized way, thereby saving the resources, reducing the production cost and greatly reducing the waste of auxiliary materials. Experimental results prove that the recovery rate of the diamond powder in the method is 81-85%.)

1. A method of extracting diamond dust from aqueous diamond fluid comprising the steps of:

A) Filtering the aqueous diamond polishing solution, and removing dental plate debris in the polishing solution;

B) Adding concentrated hydrochloric acid, stirring, standing for liquid separation, and performing suction filtration to obtain a diamond powder enrichment solution; the mass fraction of the concentrated hydrochloric acid is 20-25%;

C) Washing the diamond powder enrichment solution with deionized water, and then adding a sodium hydroxide solution for an alkalization reaction;

D) And washing the diamond powder enriched solution after the alkalization reaction by using deionized water, and then drying to obtain the diamond powder.

2. the method of claim 1, wherein step a) comprises filtering the aqueous diamond polishing solution with a 500 mesh screen.

3. the method according to claim 1, wherein the mass of the concentrated hydrochloric acid is 2 to 3 times of the mass of the aqueous diamond polishing solution filtered in the step A).

4. the method according to any one of claims 1 to 3, wherein the deionized water in the step C) has an electric conductivity of 2 to 5 μ s/cm;

The conductivity of the deionized water in the step D) is 2-5 mu s/cm.

5. The method according to claim 4, wherein the molar concentration of the sodium hydroxide solution is 2-5 mol/L.

6. the method according to claim 5, wherein the addition amount of the sodium hydroxide solution is 3-5 times of the mass of the diamond powder enriched liquid obtained after the treatment of the step B).

7. The method according to claim 6, wherein the drying temperature is 600-800 ℃;

And the drying time is 120-140 min.

8. The method of claim 1, wherein the aqueous diamond polishing solution is a waste solution of diamond and sapphire polishing on a copper plate.

9. the method of claim 7, further comprising, after step D), the steps of:

Grinding the diamond powder, screening the particle size, and packaging to obtain the finished product.

Technical Field

The invention belongs to the technical field of material preparation, and particularly relates to a method for extracting diamond powder from aqueous diamond liquid.

background

The diamond liquid has unique physical and chemical properties and is used for copper disc single-sided and double-sided copper polishing in the field of sapphire. With the development of industry, the input of various auxiliary materials and the output and the dosage of the aqueous diamond liquid are continuously increased, and the amount of the generated waste liquid is considerable but is not collected and reasonably utilized. Meanwhile, the waste liquid is polluted and wasted in the process of running away. The diamond powder is super-hard, high-wear-resistance, high-temperature-resistant and micro-powder with a large specific surface area, is expensive and is a precious resource.

Aqueous diamond liquid waste is generated by diamond liquid and sapphire in the polishing process on a copper plate. The main components of the grinding fluid are diamond powder, suspending agent, ground glass particles, copper on a copper disc and particles falling off from a dental plate. The invention is a process for removing other impurities and recovering diamond powder.

at present, the method of vibration screening is mainly adopted for the diamond powder in the aqueous diamond waste liquid, and the limitation is that diamond particles with the diameter smaller than or larger than the aperture cannot be recovered. In addition, because the cleaning process is carried out by adopting the phosphoric acid solution with the temperature of 100-200 ℃, strict requirements are imposed on a heating device and an operation process, and the steam of the phosphoric acid has quite strong corrosive action on the skin of a human body and can cause the general poisoning phenomenon.

Disclosure of Invention

The invention aims to provide a method for extracting diamond powder from aqueous diamond waste liquid, which has high recovery rate of the diamond powder and is safe and pollution-free by adopting reagents.

The invention provides a method for extracting diamond powder from aqueous diamond liquid, which comprises the following steps:

A) filtering the aqueous diamond polishing solution, and removing dental plate debris in the polishing solution;

B) adding concentrated hydrochloric acid, stirring, standing for liquid separation, and performing suction filtration to obtain a diamond powder enrichment solution; the mass fraction of the concentrated hydrochloric acid is 20-25%;

C) washing the diamond powder enrichment solution with deionized water, and then adding a sodium hydroxide solution for an alkalization reaction;

D) and washing the diamond powder enriched solution after the alkalization reaction by using deionized water, and then drying to obtain the diamond powder.

Preferably, the aqueous diamond polishing solution is filtered by a 500-mesh screen in the step a).

Preferably, the mass of the concentrated hydrochloric acid is 2-3 times of the mass of the aqueous diamond polishing solution filtered in the step A).

Preferably, the conductivity of the deionized water in the step C) is 2-5 mu s/cm;

The conductivity of the deionized water in the step D) is 2-5 mu s/cm.

preferably, the molar concentration of the sodium hydroxide solution is 2-5 mol/L.

Preferably, the addition amount of the sodium hydroxide solution is 3-5 times of the mass of the diamond powder enriched liquid obtained after the treatment in the step B).

Preferably, the drying temperature is 600-800 ℃;

And the drying time is 120-140 min.

Preferably, the aqueous diamond polishing solution is waste liquid generated by polishing diamond solution and sapphire on a copper disc.

preferably, after the step D), the method further comprises the following steps:

Grinding the diamond powder, screening the particle size, and packaging to obtain the finished product.

The invention provides a method for extracting diamond powder from aqueous diamond waste liquid, which comprises the following steps: A) filtering the aqueous diamond polishing solution, and removing dental plate debris in the polishing solution; B) adding concentrated hydrochloric acid, stirring, standing for liquid separation, and performing suction filtration to obtain a diamond powder enrichment solution; the mass fraction of the concentrated hydrochloric acid is 20-25%; C) washing the diamond powder enrichment solution with deionized water, and then adding a sodium hydroxide solution for an alkalization reaction; D) and washing the diamond powder enriched solution after the alkalization reaction by using deionized water, and then drying to obtain the diamond powder. The invention purifies the diamond powder which can be reused in the waste liquid through the processes of filtering, acidifying, washing, alkalizing to remove impurities and baking. Therefore, the waste liquid can be recycled, and can be treated in a centralized manner, so that resources are saved, the production cost is reduced, the waste of auxiliary materials can be greatly reduced, and the energy-saving and environment-friendly effects of national advocation are achieved. Experimental results prove that the recovery rate of the diamond powder in the method is 81-85%.

Detailed Description

The invention provides a method for extracting diamond powder from aqueous diamond liquid, which comprises the following steps:

A) Filtering the aqueous diamond polishing solution, and removing dental plate debris in the polishing solution;

B) Adding concentrated hydrochloric acid, stirring, standing for liquid separation, and performing suction filtration to obtain a diamond powder enrichment solution; the mass fraction of the concentrated hydrochloric acid is 20-25%;

C) washing the diamond powder enriched solution with deionized water, adding sodium hydroxide solution, and performing alkalization reaction

D) and washing the diamond powder enriched solution after the alkalization reaction by using deionized water, and then drying to obtain the diamond powder.

In the invention, the aqueous diamond polishing solution is waste liquid generated by polishing diamond solution and sapphire on a copper disc, and the waste liquid is suspension containing dental plaque waste residue, a dispersing agent, ground glass particles, copper on the copper disc and other components.

the waste liquid of the aqueous diamond liquid contains dental plate debris falling in the polishing process, and the main component of the dental plate is PVC, the particle size of PVC particles generated by a suspension method is generally 50-250 mu m, and the particle size of PVC particles generated by an emulsion method is 30-70 mu m. The PVC is present in the form of particles in an environment below 160 ℃. The invention firstly uses the filtering device to remove the dental lamina waste residue in the diamond liquid waste liquid, and the filtering device is provided with a 500-mesh screen, so that the two PVC particles can be thoroughly removed. The filtered diamond waste liquid contains components such as a dispersing agent, ground glass particles, copper on a copper disc and the like.

And then adding concentrated hydrochloric acid into the filtered diamond waste liquid, stirring for 0.5-1 hour, fully reacting, standing for 3-4 hours for liquid separation, and collecting acidified layered liquid with diamond powder enriched at the lower layer.

The mass fraction of the concentrated hydrochloric acid is preferably 20-25%, more preferably 20.24-24.1%, and most preferably 23-24.1%; the mass of the concentrated hydrochloric acid is preferably 2-3 times of the mass of the added diamond waste liquid. Concentrated hydrochloric acid dissolves copper and hydrochloric acid reacts with the alumina content of the glass particles.

and washing the collected diamond powder enrichment solution for 3-5 times by using a large amount of deionized water, wherein concentrated hydrochloric acid solution is washed, and part of dispersing agent and suspension are washed away. The conductivity of the deionized water is preferably 2-5 mu s/cm, and more preferably 3-4 mu s/cm.

And adding the diamond powder enriched solution cleaned by deionized water into a sodium hydroxide solution, further neutralizing and removing impurities. The sodium hydroxide can dissolve the alumina component in the residual sapphire glass in the solution and can also dissolve part of the reagent. The volume fraction of the sodium hydroxide solution is 5-7%, and more preferably 5-6%; the molar concentration of the sodium hydroxide solution is preferably 2-5 mol/L, and more preferably 2.5-4 mol/L; the addition amount of the sodium hydroxide solution is preferably 3-5 times of the mass of the diamond powder enriched liquid cleaned by deionized water.

And cleaning the alkalized diamond powder enrichment solution for 3-5 times by using a large amount of deionized water, wherein the conductivity of the deionized water is preferably 2-5 mus/cm, and more preferably 3-4 mus/cm.

Then covering the crucible with a crucible cover, and putting the crucible into an oven for drying to obtain diamond powder coarse powder. The baking process can completely burn impurities including organic solvent remained in the diamond liquid. The drying temperature is preferably 600-800 ℃, and more preferably 700-800 ℃; the drying time is preferably 120-140 min, and more preferably 120-130 min.

Primarily grinding the diamond powder coarse powder, collecting the diamond powder for particle size screening, quantitatively grading the diamond powder, and dividing the diamond powder into specific particle size intervals. The classification particle size was 50% classification particle size and was denoted by D50. And sticking the label and packaging to obtain the finished product.

The invention preferably screens out the diamond powder with the grain diameter of 1-2 type, 2-4 type, 3-5 type and 5-10 type, and more preferably 2-4 type.

The invention provides a method for extracting diamond powder from aqueous diamond waste liquid, which comprises the following steps: A) filtering the aqueous diamond polishing solution, and removing dental plate debris in the polishing solution; B) adding concentrated hydrochloric acid, stirring, standing for liquid separation, and performing suction filtration to obtain a diamond powder enrichment solution; the mass fraction of the concentrated hydrochloric acid is 20-25%; C) washing the diamond powder enrichment solution with deionized water, and then adding a sodium hydroxide solution for an alkalization reaction; D) and washing the diamond powder enriched solution after the alkalization reaction by using deionized water, and then drying to obtain the diamond powder. The invention purifies the diamond powder which can be reused in the waste liquid through the processes of filtering, acidifying, washing, alkalizing to remove impurities and baking. Therefore, the waste liquid can be recycled, and can be treated in a centralized manner, so that resources are saved, the production cost is reduced, the waste of auxiliary materials can be greatly reduced, and the energy-saving and environment-friendly effects of national advocation are achieved. Experimental results prove that the recovery rate of the diamond powder in the method is 81-85%, the recycling condition is good after recovery, and the cutting rate and the average yield are in accordance with requirements.

In order to further illustrate the present invention, the following examples are provided to describe the method of extracting diamond powder from aqueous diamond waste liquid, but should not be construed as limiting the scope of the present invention.