阅读说明：本技术 靶材切割研磨废液的回收方法 (Method for recovering waste liquid generated by cutting and grinding target material ) 是由 耿瑞丽 高世秀 张文涛 童培云 何坤鹏 钟小华 于 2020-12-10 设计创作，主要内容包括：本公开提供了一种靶材切割研磨废液的回收方法,其包括：将主要成分为靶材切割研磨粉料、水和切削液的靶材切割研磨废液进行固液分离,以得到切削液和水的第一混合物以及含有少量切削液和水的靶材切割研磨粉料的第二混合物；将第一混合物静置分层,上层为切削液而下层为水,将上层的切削液收集到切削液回收瓶中；将第二混合物进行旋蒸,在减压条件下采用不同的加热温度先将水蒸出、之后将切削液蒸出并收集,蒸出水和切屑液之后剩下的是靶材切割研磨粉料；将步骤三获得的靶材切割研磨粉料依次进行水洗和烘干,得到干净的靶材切割研磨粉料。由此,能对靶材切割研磨废液回收处理,进而有利于资源节约,也有利于环境保护。(The invention provides a method for recovering a target cutting and grinding waste liquid, which comprises the following steps: carrying out solid-liquid separation on the target cutting and grinding waste liquid mainly comprising target cutting and grinding powder, water and cutting fluid to obtain a first mixture of the cutting fluid and the water and a second mixture of the target cutting and grinding powder containing a small amount of the cutting fluid and the water; standing and layering the first mixture, wherein the upper layer is cutting fluid and the lower layer is water, and collecting the cutting fluid on the upper layer into a cutting fluid recovery bottle; performing rotary evaporation on the second mixture, evaporating water at different heating temperatures under reduced pressure, evaporating cutting fluid, and collecting, wherein the rest of the water and the cutting fluid is the target material cutting and grinding powder after evaporation; and D, sequentially washing and drying the target material cutting and grinding powder obtained in the step three to obtain clean target material cutting and grinding powder. Therefore, the method can recycle the waste liquid generated by cutting and grinding the target material, and is favorable for saving resources and protecting the environment.)

1. A method for recovering waste liquid generated in cutting and grinding of a target material is characterized by comprising the following steps:

the method comprises the following steps: carrying out solid-liquid separation on the target cutting and grinding waste liquid mainly comprising target cutting and grinding powder, water and cutting fluid to obtain a first mixture of the cutting fluid and the water and a second mixture of the target cutting and grinding powder containing a small amount of the cutting fluid and the water;

step two: standing and layering the first mixture, wherein the upper layer is cutting fluid and the lower layer is water, and collecting the cutting fluid on the upper layer into a cutting fluid recovery bottle;

step three: performing rotary evaporation on the second mixture, evaporating water at different heating temperatures under reduced pressure, evaporating cutting fluid, and collecting, wherein the rest of the water and the cutting fluid is the target material cutting and grinding powder after evaporation;

step four: and D, sequentially washing and drying the target material cutting and grinding powder obtained in the step three to obtain clean target material cutting and grinding powder.

2. The method for recovering the waste liquid from the cutting and grinding of the target according to claim 1,

in the first step, the cutting fluid is composed of 2-aminoethanol, 3 '-methylenebis (5-methyloxazoline) and 2, 2' -nitrilotriethanol,

based on the total weight of the cutting fluid: 20-30% of 2-aminoethanol, 30-40% of 3,3 '-methylenebis (5-methyl oxazoline) and 30-40% of 2, 2' -nitrilotriethanol.

3. The method for recovering the waste liquid from the cutting and grinding of the target according to claim 1,

in the first step, centrifugal separation is adopted for solid-liquid separation.

4. The method for recovering the waste liquid from the cutting and grinding of the target according to claim 1,

and in the second step, standing for 10-30 min.

5. The method for recovering the waste liquid from the cutting and grinding of the target according to claim 1,

and in the second step, collecting the cutting fluid on the upper layer into a beaker, adding anhydrous sodium sulfate and/or anhydrous magnesium sulfate into the beaker, standing, and collecting the cutting fluid into a cutting fluid recovery bottle.

6. The method for recovering the waste liquid from the cutting and grinding of the target according to claim 5,

in the second step, the amount of the anhydrous sodium sulfate and/or anhydrous magnesium sulfate added is 0.2 to 2% by mass of the first mixture.

7. The method for recovering the waste liquid from the cutting and grinding of the target according to claim 5,

standing for 10-30 min.

8. The method for recovering the waste liquid from the cutting and grinding of the target according to claim 1,

in the third step, the pressure reduction condition is 55Pa to 100Pa, the heating temperature of the distilled water is 50 ℃ to 60 ℃, and the heating temperature of the distilled cutting fluid is 65 ℃ to 85 ℃.

9. The method for recovering the waste liquid from the cutting and grinding of the target according to claim 1,

in the fourth step, the water washing is carried out for 2 to 5 times by adopting deionized water.

10. The method for recovering the waste liquid from the cutting and grinding of the target according to claim 1,

in the fourth step, the drying temperature is 60-80 ℃, and the drying time is 3-5 h.

Technical Field

The disclosure relates to the field of targets, and more particularly relates to a method for recovering a target cutting and grinding waste liquid.

Background

The target material is a target material bombarded by high-speed charged energy particles. It is well known that the technological development trend of target materials is closely related to the development trend of thin film technology in downstream application industries. As the application industry has improved on thin film products or devices, the target technology should also change.

In the application process of the target material, the target material needs to be cut, ground and processed into a proper size. And generating target cutting and grinding waste liquid in the cutting and grinding process, wherein the target cutting and grinding waste liquid contains cutting fluid, water and a certain amount of target cutting and grinding powder.

The waste liquid generated by cutting and grinding the target material is recycled, so that the resource saving and the environmental protection are facilitated.

Disclosure of Invention

In view of the problems in the background art, an object of the present disclosure is to provide a method for recovering a waste liquid from cutting and grinding of a target, which can recover and treat the waste liquid from cutting and grinding of the target, thereby saving resources and protecting the environment.

In order to achieve the above object, the present disclosure provides a method for recovering a waste liquid from cutting and grinding of a target, comprising the steps of: the method comprises the following steps: carrying out solid-liquid separation on the target cutting and grinding waste liquid mainly comprising target cutting and grinding powder, water and cutting fluid to obtain a first mixture of the cutting fluid and the water and a second mixture of the target cutting and grinding powder containing a small amount of the cutting fluid and the water; step two: standing and layering the first mixture, wherein the upper layer is cutting fluid and the lower layer is water, and collecting the cutting fluid on the upper layer into a cutting fluid recovery bottle; step three: performing rotary evaporation on the second mixture, evaporating water at different heating temperatures under reduced pressure, evaporating cutting fluid, and collecting, wherein the rest of the water and the cutting fluid is the target material cutting and grinding powder after evaporation; step four: and D, sequentially washing and drying the target material cutting and grinding powder obtained in the step three to obtain clean target material cutting and grinding powder.

In some embodiments, in step one, the composition of the cutting fluid is 2-aminoethanol, 3 '-methylenebis (5-methyloxazoline), 2', 2 "-nitrilotriethanol, based on the total weight of the cutting fluid: 20-30% of 2-aminoethanol, 30-40% of 3,3 '-methylenebis (5-methyl oxazoline) and 30-40% of 2, 2' -nitrilotriethanol.

In some embodiments, in step one, the solid-liquid separation is performed by centrifugation.

In some embodiments, in step two, the mixture is allowed to stand for 10min to 30 min.

In some embodiments, in the second step, the cutting fluid in the upper layer is collected into a beaker, then anhydrous sodium sulfate and/or anhydrous magnesium sulfate is added into the beaker, after standing, the cutting fluid is collected into a cutting fluid recovery bottle, and the anhydrous sodium sulfate and/or anhydrous magnesium sulfate after absorbing water is collected, dried and reused. In some embodiments, the amount of anhydrous sodium sulfate and/or anhydrous magnesium sulfate added is 0.2% to 2% by mass of the first mixture. In some embodiments, the time of standing is 10min to 30 min.

In some embodiments, in the third step, the pressure reduction condition is 55Pa to 100Pa, the heating temperature of the distilled water is 50 ℃ to 60 ℃, and the heating temperature of the distilled cutting fluid is 65 ℃ to 85 ℃.

In some embodiments, in step four, the water wash is 2-5 washes with deionized water.

In some embodiments, in the fourth step, the drying temperature is 60 ℃ to 80 ℃, and the drying time is 3h to 5 h.

The beneficial effects of this disclosure are as follows: in the method for recovering the waste cutting and grinding liquid of the target material, the second step is used for separating and recovering the cutting liquid from the first mixture, and the third step is used for separating water, the cutting liquid and the target material cutting and grinding powder from the second mixture, so that the waste cutting and grinding liquid of the target material can be recovered, resources can be saved, and environmental protection can be facilitated.

Detailed Description

The method for recovering the waste cutting and polishing solution of the target material of the present disclosure will be described in detail below.

The method for recovering the waste liquid generated by cutting and grinding the target material comprises the following steps: the method comprises the following steps: carrying out solid-liquid separation on the target cutting and grinding waste liquid mainly comprising target cutting and grinding powder, water and cutting fluid to obtain a first mixture of the cutting fluid and the water and a second mixture of the target cutting and grinding powder containing a small amount of the cutting fluid and the water; step two: standing and layering the first mixture, wherein the upper layer is cutting fluid and the lower layer is water, and collecting the cutting fluid on the upper layer into a cutting fluid recovery bottle; step three: performing rotary evaporation on the second mixture, evaporating water at different heating temperatures under reduced pressure, evaporating cutting fluid, and collecting, wherein the rest of the target material cutting and grinding powder is left after the water and the cutting fluid are evaporated; step four: and D, sequentially washing and drying the target material cutting and grinding powder obtained in the step three to obtain clean target material cutting and grinding powder.

In some embodiments, in step one, the water is deionized water. The introduction of impurities can be reduced by using deionized water.

In some embodiments, in step one, the composition of the cutting fluid is 2-aminoethanol, 3 '-methylenebis (5-methyloxazoline), 2', 2 "-nitrilotriethanol, based on the total weight of the cutting fluid: 20-30% of 2-aminoethanol; 30-40% of 3, 3' -methylenebis (5-methyl oxazoline); the content of 2, 2' -nitrilotriethanol is 30-40%.

In some embodiments, in step one, the target-cut abrasive is a target-cut abrasive of ITO, GZO, or IGZO. Of course, the method is not limited thereto, and may be applied to other suitable target cutting abrasive powders, such as AZO and ATO.

In some embodiments, in step one, the solid-liquid separation is performed by centrifugation. Compared with standing, centrifugal separation needs to enable the cutting fluid and water to be thoroughly separated from the target material cutting and grinding powder, so that automatic operation is facilitated, and working efficiency is improved.

In some embodiments, in step two, the standing time is from 10min to 30 min. The standing time is less than 10min, so that the layering is incomplete, and the recovery rate of the cutting fluid is reduced; the standing time is more than 30min, which is not beneficial to improving the working efficiency.

In some embodiments, in the second step, the cutting fluid in the upper layer is collected into a beaker, then anhydrous sodium sulfate or anhydrous magnesium sulfate is added into the beaker to remove a small amount of water in the cutting fluid, the cutting fluid is collected into a cutting fluid recovery bottle after standing, and the anhydrous sodium sulfate and/or anhydrous magnesium sulfate after absorbing water is collected, dried and reused. In some embodiments, the time of standing is 10min to 30 min. Standing for less than 10min, and removing water by anhydrous sodium sulfate or anhydrous magnesium sulfate; the standing time is more than 30min, which is not beneficial to improving the working efficiency. In some embodiments, the anhydrous sodium sulfate and/or anhydrous magnesium sulfate is added in an amount of 0.2% to 2% by mass of the first mixture.

In the second step, in the above embodiment, the separation and recovery of the cutting fluid from the first mixture is achieved.

In the third step, rotary evaporation is adopted to realize the separation of water, the cutting fluid and the target cutting and grinding powder from the second mixture, and the cutting fluid and the target cutting and grinding powder are recovered.

In the third step, the pressure reduction condition is 55Pa to 100Pa, the heating temperature of the distilled water is 50 ℃ to 60 ℃, and the heating temperature of the distilled cutting fluid is 65 ℃ to 85 ℃. Under the reduced pressure condition, the boiling points of the water and the cutting fluid components are lower than the boiling point under normal atmospheric pressure, so that the target cutting and grinding powder can be separated from the water and the cutting fluid by using a reduced pressure distillation method.

Collecting the water evaporated in the third step into a liquid collecting bottle, and collecting the cutting fluid evaporated in the second step into another liquid collecting bottle.

In some embodiments, in step four, the water wash is 2-5 washes with deionized water. The adoption of deionized water can prevent impurity pollution.

In some embodiments, in the fourth step, the drying temperature is 60 ℃ to 80 ℃, and the drying time is 1h to 4 h.

Finally, a test process is given.

In the following examples, the main components of the waste target cutting and grinding liquid are target cutting and grinding powder, water and cutting liquid, wherein the water is deionized water, and the composition of the cutting liquid is: based on the total weight of the cutting fluid, the content of 2-aminoethanol is 26%, the content of 3,3 '-methylenebis (5-methyloxazoline) is 37%, and the content of 2, 2' -nitrilotriethanol is 37%.

Example 1

The method comprises the following steps: taking ITO (In)₂O₃:SnO₂90:10, wt%) of 2Kg of waste cutting and grinding liquid of the target material, and centrifugally separating the waste cutting and grinding liquid of the ITO target material to obtain 0.42Kg of first mixture of cutting liquid and water and 1.58Kg of second mixture of cutting and grinding powder containing a small amount of cutting liquid and water;

step two: putting the first mixture obtained in the step one into a pear-shaped separating funnel, standing for 15min for layering, collecting 0.31Kg of cutting fluid on the upper layer into a beaker, adding 3g of anhydrous sodium sulfate into the beaker, standing for 30min, transferring the cutting fluid into a cutting fluid recovery bottle, collecting, drying and reusing the anhydrous sodium sulfate after absorbing water;

step three: putting the second mixture obtained in the step one into a single-neck round-bottom flask (the volume is 1L, and the charging amount is less than half of the volume of the flask) for rotary evaporation, evaporating 23mL of water at the vacuum degree of 80Pa and the heating temperature of 55 ℃ and collecting the water into a liquid collecting bottle, then replacing the liquid collecting bottle, setting the heating temperature to 70 ℃ and the vacuum degree to 80Pa, evaporating 18mL of cutting fluid and collecting the cutting fluid into the liquid collecting bottle, wherein 1.54Kg of ITO cutting grinding powder is in the single-neck round-bottom flask;

step four: and (4) washing the ITO cutting grinding powder obtained in the step three with deionized water for three times, and then drying at the drying temperature of 70 ℃ for 4 hours to obtain clean ITO cutting grinding powder.

Example 2

The method comprises the following steps: taking GZO (ZnO: Ga)₂O₃97:3, wt%) of the waste cutting and grinding target material, performing centrifugal separation on the waste cutting and grinding target material, and separating to obtain 0.53Kg of a first mixture of cutting fluid and water and 1.47Kg of a second mixture of cutting and grinding powder containing a small amount of cutting fluid and water;

step two: putting the first mixture obtained in the step one into a pear-shaped separating funnel, standing for 10min for layering, collecting 0.42Kg of cutting fluid on the upper layer and water on the lower layer into a beaker, adding 1.1g of anhydrous sodium sulfate into the beaker, standing for 30min, collecting the cutting fluid into a cutting fluid recovery bottle, collecting, drying and reusing the anhydrous sodium sulfate after water absorption;

step three: putting the second mixture obtained in the first step into a single-neck round-bottom flask (the volume is 1L, and the charging amount is less than half of the volume of the flask) for rotary evaporation, evaporating 29mL of water at the vacuum degree of 55Pa and the heating temperature of 50 ℃ and collecting the water into a liquid collecting bottle, then replacing the liquid collecting bottle, setting the heating temperature to 65 ℃ and the vacuum degree of 55Pa, evaporating 22mL of cutting fluid and collecting the cutting fluid into the liquid collecting bottle, wherein 1.42Kg of GZO cutting ground powder is in the single-neck round-bottom flask;

step four: and (3) washing the GZO cutting and grinding powder obtained in the step three with deionized water twice, and then drying at the drying temperature of 60 ℃ for 5 hours to obtain clean GZO cutting and grinding powder.

Example 3

The method comprises the following steps: taking IGZO (In)₂O₃:Ga₂O₃ZnO is 1:1:1, wt%) and 2Kg of waste cutting and grinding liquid of the target material, the waste cutting and grinding liquid of the IGZO target material is centrifugally separated to obtain 0.49Kg of a first mixture of cutting liquid and water and 1.51Kg of a second mixture of cutting and grinding powder containing a small amount of cutting liquid and water;

step two: putting the first mixture obtained in the step one into a pear-shaped separating funnel, standing for 20min for layering, wherein the upper layer is cutting fluid and the lower layer is water, collecting 0.35Kg of cutting fluid on the upper layer into a beaker, recovering water on the lower layer, adding 9.8g of anhydrous sodium sulfate into the beaker, standing for 30min, collecting the cutting fluid into a cutting fluid recovery bottle, and collecting, drying and reusing the anhydrous sodium sulfate after water absorption;

step three: filling the second mixture obtained in the step one into a single-neck round-bottom flask (the volume is 1L, and the charging amount is less than half of the volume of the flask) for rotary evaporation, wherein the vacuum degree is 100Pa, the heating temperature is 60 ℃, 26mL of water is distilled out and collected into a liquid collecting bottle, then the liquid collecting bottle is replaced, the heating temperature is 85 ℃, the vacuum degree is 100Pa, 20mL of cutting fluid is distilled out and collected into the liquid collecting bottle, and 1.46Kg of IGZO cutting grinding powder is filled in the single-neck round-bottom flask;

step four: washing the IGZO cutting and grinding powder obtained in the third step twice by using deionized water, and then drying at the drying temperature of 80 ℃ for 3h to obtain clean IGZO cutting and grinding powder.