Method for cleaning quartz glass of adhering iron oxides and electric soot

Abstract

The application discloses a quartz glass attached iron oxide and electric fire ash cleaning method and belongs to the detection field, and comprises the following steps: S1, physical cleaning; 2, primary acid dissolution; 3, secondary acid dissolution; S4, reductive acid dissolution; S5, weak acid dissolution; S6, ethanol ultrasonic cleaning; and S7, drying. Compared with the prior art, the method has the characteristics of reliable cleaning and no damage to the body.

Description

TECHNICAL FIELD

[0001] The present application relates to a cleaning method, in particular to a cleaning method suitable for cleaning iron oxide and electric spark ash attached to quartz glass. BACKGROUND

[0002] The ARL4460 photoelectric direct-reading spectrometer is equipped with an insulating quartz dust collection cup for electric spark insulation and isolation excitation of waste (iron oxide, electric spark ash impurities). During use, iron oxide and electric spark ash impurities are attached to the body of the insulating quartz dust collection cup at high temperature, and when accumulated to a certain extent, the function gradually fails, the device failure rate increases, the test accuracy decreases, and it must be replaced.

[0003] The insulating quartz dust collection cup is a special spare part for precision instruments, which is a non-standard imported part of foreign patent, and the market price is about 8500 yuan per unit. An insulating quartz dust collection cup needs to be replaced when the ARL4460 photoelectric direct-reading spectrometer is excited about 40-50 thousand times on average, and the replacement cost is high.

[0004] The substrate of the insulating quartz dust collection cup is quartz glass, and the raw material of the quartz glass is silicon tetrachloride (SiCl4). In the prior art, the surface of the quartz glass is usually cleaned by chemical, physical or mechanical methods. The structure of the insulating quartz dust collection cup is complex, so the physical or mechanical methods suitable for flat pieces or quartz glass rods cannot be used for reference. As for the chemical method, most of the existing cleaning methods for quartz glass are intended to roughen the surface to facilitate the next step of coating or coating, such as the RCA method (acidic hydrogen peroxide prepared by concentrated sulfuric acid for acidic oxidation flushing), and some schemes even use 10% to 20% hydrofluoric acid solution for immersion. The above methods will cause hydrogen embrittlement in the quartz glass, damage the raw materials, and destroy the transparency, purity, surface smoothness, etc., resulting in a decrease in the accuracy of the equipment when reused. Other relatively mild cleaning methods, such as a quartz glass cleaning method (CN201510468665.X), are suitable for removing rubber contamination. The cleaning solution disclosed in a cleaning method for quartz glass substrate for total reflection X-ray fluorescence analysis (CN201610695658.8) is a potassium permanganate sulfuric acid solution, wherein the concentration of potassium permanganate is 4-6wt%; the volume concentration of sulfuric acid in the potassium permanganate sulfuric acid solution is 8-12%; and it is suitable for cleaning the residual Cr element on the quartz glass substrate. However, it does not solve the problem of iron oxide (ferric oxide, ferrous oxide, magnetite, etc.) and electric spark ash impurities (carbon, carbonate) attached at high temperature.

[0005] Based on the above technical difficulties, there is currently no cleaning and recycling method for the insulating quartz dust collection cup of the device in the domestic steel industry after it is discarded, and the procurement quantity is large. Therefore, a method for completely cleaning the iron oxide and electric spark ash impurities attached to the insulating quartz dust collection cup at high temperature is urgently needed to realize recycling and reduce costs and increase efficiency. Summary of the Invention

[0006] The technical objective of this invention is to address the shortcomings of the prior art by providing a method for cleaning iron oxides and electrolytic ash adhering to quartz glass, thoroughly cleaning away iron oxides and electrolytic ash impurities adhering to the insulating quartz dust collection cup, extending the service life of the insulating quartz dust collection cup, reducing costs, and ensuring the accuracy of related precision instruments.

[0007] The technical solution of this invention to solve its technical problem is: a method for cleaning iron oxides and electrostatic ash adhering to quartz glass, characterized by including the following steps:

[0008] S1, Physical Cleaning

[0009] S2, Initial acid dissolution: Mix high-concentration strong acid and water at a volume ratio of 1:2, immerse the waste insulating quartz dust collection cup treated by S1 in the solution and let it stand. Environmental conditions: temperature 25±5℃, time 12~24 hours.

[0010] S3, Secondary Acid Dissolution: High-concentration strong acid and water are mixed at a volume ratio of 1:3. The waste insulating quartz dust collection cup treated by S2 is immersed in the ultrasonic cleaner. The environmental conditions are: 50±5℃, vibration frequency 40~60KHz, time 30~60min.

[0011] S4. Dissolving with reducing acid: Immerse the waste insulating quartz dust collection cup treated with S3 in reducing acid and let it stand. Environmental conditions: temperature 25±5℃, time 10~12 hours.

[0012] S5. Weak acid dissolution: Immerse the waste insulating quartz dust collection cup treated with S4 in a weak acid and let it stand. Environmental conditions: temperature 25±5℃, time 12~24 hours.

[0013] S6, Ethanol Ultrasonic Cleaning: Immerse the waste insulating quartz dust collection cup treated with S5 in ethanol and treat it with an ultrasonic cleaner. Environmental conditions: 25±5℃, vibration frequency 40~60KHz, time 20~40min.

[0014] S7. Drying.

[0015] Furthermore, in the above-mentioned physical cleaning S1: brushing with a brush followed by rinsing; after rinsing, placing it in an ultrasonic cleaner for treatment, with environmental conditions of: temperature 25±5℃, vibration frequency 40~60KHz, and time 10~20min.

[0016] Furthermore, the rinsing solution mentioned above is ethanol.

[0017] Furthermore, the aforementioned high-concentration strong acid is one of concentrated hydrochloric acid, concentrated sulfuric acid, or concentrated nitric acid.

[0018] Further, the high concentration strong acid used in the above-mentioned S1 primary acid dissolution and S2 secondary acid dissolution is the same in type and concentration.

[0019] Further, in the above-mentioned S1 primary acid dissolution and S2 secondary acid dissolution, the acid dissolution is completed and then washed with water.

[0020] Further, the above-mentioned reducing acid is one of oxalic acid and formic acid.

[0021] Further, the above-mentioned weak acid is acetic acid or other weak acid with a PH value in the range of 4.0-6.0.

[0022] Further, the above-mentioned drying is placed in the backlight and dried.

[0023] Compared with the prior art, the present application has the following outstanding beneficial effects:

[0024] 1. The method can completely clean the iron oxide and electric soot impurities attached to the insulating quartz dust collecting cup, so that the insulating quartz dust collecting cup can be recycled to prolong the service life of the insulating quartz dust collecting cup, reduce the replacement frequency of new products, and reduce the cost.

[0025] 2. The method does not harm the raw materials, and the transparency, purity, surface smoothness, etc. are equivalent to new products, and the recycling does not affect the equipment precision.

[0026] 3. The method can clean the insulating dust collecting cup regularly according to the actual situation, maintain the sustained good performance of the insulating dust collecting cup, make it can play a more lasting function, and prolong the service life or increase the recycling times of the product. BRIEF DESCRIPTION OF DRAWINGS

[0027] Figure 1 is a comparison diagram before and after cleaning of the present application.

[0028] Figure 2 is a comparison diagram before and after cleaning of the comparative example.

[0029] Figure 3 is a sample detection data table after treatment of the example and the comparative example. DETAILED DESCRIPTION

[0030] The present application will be further described below in combination with the drawings and specific embodiments.

[0031] For purposes of the following detailed description, it is to be understood that the application can assume various alternative variations and step sequences, except where expressly specified to the contrary, and that the described implementation is done only by way of example and not as an limitation of the application. In addition, all numerical values are to be understood as modified in all instances by the term "about," unless otherwise specifically noted. At least, and without intent to limit the application's scope to equivalents, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.

[0032] Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the application are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements.

[0033] It also should be understood that any numerical range recited herein is intended to include all sub-ranges subsumed therein. For example, a range of "1 to 10" is intended to include all sub-ranges, for example, from the minimum "1" to any other number less than "10", for example, "1 to 6," "3 to 7," "5 to 9," or "5 to 6," to the maximum "10." In other words, every single value within the indicated range is intended to be included.

[0034] In this application, the use of the singular includes the plural, and vice versa, unless specifically stated otherwise. Also, in this application, the use of "or" means "and / or" unless stated otherwise, even though "and / or" can be explicitly used in certain instances. Further, in this application, the use of "one" or "a" means "at least one", unless specifically stated otherwise. For example, "an" first material, "a" coating composition, and the like, means one or more items of these items.

[0035] The present application is a method for cleaning quartz glass adhered iron oxide and electric fire ash, which is used to completely clean the iron oxide (ferric oxide, ferrous oxide, magnetite, etc.) and electric fire ash impurities (carbon, carbonate) adhered to quartz glass at high temperature.

[0036] The method of the present application, the specific steps include:

[0037] S1, physical cleaning

[0038] (1) Brush the waste insulation quartz integrated cup with a brush, and then rinse it with anhydrous ethanol (CH3CH2OH≧99.5%);

[0039] (2) Put it into an ultrasonic cleaner for processing, and the environmental conditions are: temperature 25±5℃, vibration frequency 40-60KHz, and time 10-20min.

[0040] This step removes the weakly adhering particles and other impurities by purely physical methods.

[0041] S2, primary acid dissolution

[0042] (1) High-concentration strong acid and water are mixed at a ratio of 1:2 by volume, and the waste and used insulating quartz dust collecting cups treated in S1 are immersed and left to stand, with the environmental conditions being a temperature of 25±5°C and a time of 12-24 hours. The high-concentration strong acid is one of concentrated hydrochloric acid (HCl: 36.0%-38.0%), concentrated sulfuric acid (H2SO4: 70%-99%), and concentrated nitric acid (HNO3: 68%-75%);

[0043] (2) After completion, the cups are washed with water.

[0044] This step uses a relatively strong acidic solution to dissolve the rough iron oxide and small amounts of electric fire ash adhering to the surface of the insulating quartz dust collecting cups by chemical methods. In specific implementation, 5 dust collecting cups can be treated per 1000 milliliters of solution.

[0045] S3, secondary acid dissolution

[0046] (1) High-concentration strong acid and water are mixed at a ratio of 1:3 by volume, and the waste and used insulating quartz dust collecting cups treated in S2 are immersed and treated in an ultrasonic cleaning machine, with the environmental conditions being a temperature of 50±5°C, a vibration frequency of 40-60 KHz, and a time of 30-60 minutes. The high-concentration strong acid is the same as in S2 in terms of type and concentration.

[0047] (2) After completion, the cups are washed with water.

[0048] This step weakens the effect of acid dissolution and strengthens the physical conditions, removing some remaining stubborn iron oxide and sporadic electric fire ash impurities in a relatively short time, and avoiding damage to the surface layer of the quartz integrated cup.

[0049] S4, reducing acid dissolution

[0050] The waste and used insulating quartz dust collecting cups treated in S3 are immersed and left to stand in a reducing acid (concentration ≧99.5%), with the environmental conditions being a temperature of 25±5°C and a time of 10-12 hours. The reducing acid is one of oxalic acid and formic acid.

[0051] This process uses the reducing property of oxalic acid to reduce the remaining trivalent iron that cannot be dissolved into easily soluble divalent iron through a slow reaction, and then dissolves the divalent iron through complexation with oxalic acid. This process treats trace amounts of residual iron ion substances.

[0052] S5, weak acid dissolution

[0053] S4, the waste insulation quartz dust cup is immersed in weak acid (concentration ≧99.5%) and is placed for 12-24 hours under the environmental condition of 25±5℃. The weak acid is acetic acid or other weak acid with PH value in the range of 4.0-6.0.

[0054] This process dissolves the residual iron oxide by using a relatively mild acid and avoids damaging the surface layer of the dust cup.

[0055] S6, ethanol ultrasonic cleaning

[0056] The waste insulation quartz dust cup treated by S5 is immersed in ethanol (purity >99.5%) and is treated by an ultrasonic cleaning machine under the environmental condition of 25±5℃, vibration frequency 40-60KHz and time 20-40min.

[0057] This step rinses the acid solution and removes the possible impurities that are insoluble in acid and water.

[0058] S7, drying

[0059] The waste insulation quartz dust cup treated by S5 is placed in a back light place and is used after being dried.

[0060] In order to better compare the method of the present application and the prior art, a comparative test is carried out.

[0061] The control group adopts gradient acid dissolution, and the specific steps are as follows:

[0062] S1, physical cleaning, same as the process of the present application.

[0063] S2, first acid dissolution: the waste insulation quartz dust cup treated by S1 is immersed in concentrated hydrochloric acid and water (volume ratio 1:2) and is placed for 24 hours at room temperature; and then is cleaned with water;

[0064] S3, second acid dissolution: the waste insulation quartz dust cup treated by S2 is immersed in concentrated hydrochloric acid and water (volume ratio 1:3) and is placed for 12 hours at room temperature; and then is cleaned with water;

[0065] S4, third acid dissolution: the waste insulation quartz dust cup treated by S3 is immersed in concentrated hydrochloric acid and water (volume ratio 1:4) and is placed for 12 hours at room temperature; and then is cleaned with water;

[0066] S5, fourth acid dissolution: the waste insulation quartz dust cup treated by S4 is immersed in concentrated hydrochloric acid and water (volume ratio 1:5) and is placed for 12 hours at room temperature; and then is cleaned with water;

[0067] S6, ethanol ultrasonic cleaning: same as the process of the present application.

[0068] S7, drying: same as the process of the present application.

[0069] The dust collecting cup using the embodiment of the method of the application and the control group dust collecting cup using the gradient acid dissolution method are used to detect five samples with different gradients of ingredient content, and the comparison result table is shown in Figure 3 From the above results, it can be seen that the data deviation of the five elements (carbon, silicon, manganese, phosphorus and sulfur) of the dust collecting cup cleaned by the method of the application before and after cleaning does not exceed the national standard allowable deviation, while after the dust collecting cup treated by the gradient acid dissolution method detects the same five samples, one item of data exceeds the national standard deviation, and the sum of the absolute value differences of the five samples is greater than the result after the former method, and the stability is poor.

[0070] From the above results, it can be seen that the method of the application can completely clean the iron oxide and electric ash impurities attached to the insulating quartz dust collecting cup, so that the insulating quartz dust collecting cup can be recycled to prolong the service life of the insulating quartz dust collecting cup, reduce the replacement frequency of new products, and reduce the cost; and does not harm the raw materials, and the transparency, purity, surface smoothness, etc. are equivalent to new products, and do not affect the equipment precision when reused.

[0071] It should be noted that the specific embodiments of the application have been described in detail, and various obvious changes made by those skilled in the art without departing from the spirit and scope of the application are within the protection scope of the application.

Claims

1. A method for cleaning iron oxides and electrostatic ash adhering to quartz glass, characterized in that: Includes the following steps, S1. Physical cleaning; S2, Initial acid dissolution: Mix high-concentration strong acid and water at a volume ratio of 1:2, immerse the waste insulating quartz dust collection cup treated by S1 in the solution and let it stand. Environmental conditions: temperature 25±5℃, time 12~24 hours. S3, Secondary Acid Dissolution: High-concentration strong acid and water are mixed at a volume ratio of 1:

3. The waste insulating quartz dust collection cup treated by S2 is immersed in the ultrasonic cleaner. The environmental conditions are: 50±5℃, vibration frequency 40~60KHz, time 30~60min. S4. Dissolving with reducing acid: Immerse the waste insulating quartz dust collection cup treated in S3 in a reducing acid and let it stand. The reducing acid is either oxalic acid or formic acid. Environmental conditions: temperature 25±5℃, time 10~12 hours. S5. Weak acid dissolution: Immerse the waste insulating quartz dust collection cup treated with S4 in a weak acid and let it stand. Environmental conditions: temperature 25±5℃, time 12~24 hours. S6, Ethanol Ultrasonic Cleaning: Immerse the waste insulating quartz dust collection cup treated with S5 in ethanol and treat it with an ultrasonic cleaner. Environmental conditions: 25±5℃, vibration frequency 40~60KHz, time 20~40min. S7. Drying.

2. The method for cleaning iron oxides and electrostatic ash adhering to quartz glass according to claim 1, characterized in that: In the S1 physical cleaning process: brushing with a brush followed by rinsing; after rinsing, placing the device in an ultrasonic cleaner for treatment under the following environmental conditions: temperature 25±5℃, vibration frequency 40~60KHz, and time 10~20min.

3. The method for cleaning iron oxides and electrostatic ash adhering to quartz glass according to claim 2, characterized in that: The rinsing solution is ethanol.

4. The method for cleaning iron oxides and electrostatic ash adhering to quartz glass according to claim 1, characterized in that: The high-concentration strong acid is one of concentrated hydrochloric acid, concentrated sulfuric acid, or concentrated nitric acid.

5. The method for cleaning iron oxides and electrostatic ash adhering to quartz glass according to claim 1, characterized in that: The high-concentration strong acid used in the initial acid dissolution (S2) and the secondary acid dissolution (S3) is of the same type and concentration.

6. The method for cleaning iron oxides and electrostatic ash adhering to quartz glass according to claim 1, characterized in that: In the initial acid dissolution (S2) and secondary acid dissolution (S3), the solution is washed with water after the acid dissolution is completed.

7. The method for cleaning iron oxides and electrostatic ash adhering to quartz glass according to claim 1, characterized in that: The weak acid is acetic acid or other weak acids with a pH value in the range of 4.0 to 6.

0.

8. The method for cleaning iron oxides and electrostatic ash adhering to quartz glass according to claim 1, characterized in that: The drying process involves placing the item in a shaded area to air dry.

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