WO2017030282A1 - Over-descaling preventive agent analyzing apparatus and over-descaling preventive agent analyzing method using same - Google Patents

Abstract

Disclosed are an over-descaling preventive agent analyzing apparatus and an over-descaling preventive agent analyzing method using the same. According to an embodiment, the over-descaling preventive agent analyzing apparatus comprises: a first reaction part including a first inlet unit, a second inlet unit, a third inlet unit, and a fourth inlet unit; a second reaction part including a fifth inlet unit, a sixth inlet unit, a seventh inlet unit, a pH measurement unit, and a level measurement unit; and a control and operation part electrically connected with the pH measurement unit and the level measurement unit.

Description

Device for Analyzing Anti-Ocean Tax and Method for Analyzing Anti-Ocean Tax Using the Same

The present invention relates to an anti-acid tax inhibitor analysis apparatus and a method for analyzing the anti-acid tax inhibitor using the same. More specifically, the present invention relates to a concentration analysis device for the amine-based compound included in the anti-acid pickling inhibitor used in the pickling rolling process in the production of cold rolled steel sheets, and a method for analyzing the anti-acid pickling agent using the same.

The cold rolling process is a step of rolling a hot rolled steel at a temperature near room temperature, and is a step of producing a product having a beautiful surface and excellent workability. In the cold rolling process, the hot rolled coil is subjected to a pickling and rolling facility, and then the final product is produced through a facility such as galvanizing or cold rolling.

In the pickling rolling equipment, the oxides attached to the surface of the hot-rolled steel sheet are pickled and then continuously rolled to a desired thickness at room temperature to produce a semi-finished product, in which hydrochloric acid is used for pickling.

Background art related to the present invention is disclosed in Korean Unexamined Patent Publication No. 2004-0017751 (published on Feb. 27, 2004, titled invention: Pickling method of hot rolled steel sheet).

According to one embodiment of the present invention, to provide an anti-acid tax inhibitor analysis device having excellent reliability, accuracy and precision.

According to an embodiment of the present invention, it is to provide an anti-acid detergent analysis device excellent in preventing the surface acid wash of the cold rolled steel sheet to prevent the surface failure.

According to one embodiment of the present invention, to provide an anti-acid pickling agent analysis device that can improve the work efficiency during the pickling process.

According to one embodiment of the present invention, to provide an anti-acid tax inhibitor analysis method using the anti-acid tax inhibitor analysis apparatus.

One aspect of the present invention relates to an anti-acid tax inhibitor. In one embodiment, the anti-acid tax inhibitor analysis device, the first inlet portion, the second inlet portion is introduced, the decomposition agent is introduced into the anti-acid detergent including an amine-based compound, SHST (sodium hydroxide-sodium thiosulfate) solution is introduced A third inlet and a fourth inlet through which water is introduced are provided, wherein a decomposing agent is added to the anti-acid pickling agent and heated to decompose the anti-acid pickling agent, and the SHST solution and water are introduced into the decomposed anti-acid pickling agent. And distillation to generate ammonia (NH ₃ ); A fifth inlet for introducing ammonia distilled from the first reaction unit and a sixth inlet for introducing boric acid; And a seventh inflow portion into which sulfuric acid flows in, a pH measuring portion measuring internal pH, and a level measuring portion measuring internal level, collecting the introduced ammonia with boric acid to generate a collection solution, and introducing the sulfuric acid to the A second reaction unit for titrating the collection solution; And a control operation unit electrically connected to the pH measuring unit and the level measuring unit to transmit the measured pH and level data inside the second reaction unit to analyze the concentration of the anti-acid tax inhibitor.

Another aspect of the present invention relates to a method of analyzing the anti-acid tax inhibitor using the apparatus for analyzing the anti-acid tax inhibitor. In one embodiment, the method for analyzing the anti-acid detergent comprises adding a decomposing agent to the anti-acid detergent including the amine compound and heating the decomposition. Collecting ammonia (NH ₃ ) generated by adding a sodium hydroxide-sodium thiosulfate (SHST) solution and water to the decomposed anti-acid detergent; Collecting the collected ammonia (NH ₃ ) with boric acid to generate a collection solution; And titrating the collection solution with sulfuric acid to derive the nitrogen concentration contained in the ammonia (NH ₃ ), wherein the decomposition agent includes potassium sulfate (K ₂ SO ₄ ), copper sulfate (CuSO ₄ ), and sulfuric acid. It is prepared by mixing (H ₂ SO ₄ ) and water.

In one embodiment, the heating may be performed at 350 ℃ ~ 400 ℃.

In one embodiment the distillation may be performed at 60 ℃ ~ 100 ℃.

In one embodiment said titration comprises measuring the pH of said boric acid; And adding sulfuric acid to the collection solution, adjusting the pH of the collection solution to the pH of the measured boric acid.

When applying the method of analyzing the anti-acid tax inhibitor of the present invention, the measurement reliability, accuracy and precision of the concentration of the amine-based compound contained in the anti-acid tax inhibitor is excellent, and it is excellent in preventing the surface acid wash of the cold rolled steel sheet, thereby preventing the surface defects. The work efficiency can be improved in the pickling process.

Figure 1 shows an analysis device for anti-acid tax inhibitor according to an embodiment of the present invention.

Figure 2 shows the analysis method of the anti-acid tax inhibitor according to an embodiment of the present invention.

Figure 3 is a graph comparing the concentration of the amine compound contained in the prepared anti-acid inhibitor and the measured anti-acid detergent.

In the following description of the present invention, when it is determined that detailed descriptions of related well-known technologies or configurations may unnecessarily obscure the subject matter of the present invention, the detailed description will be omitted.

The terms to be described below are terms defined in consideration of functions in the present invention, and may be changed according to intentions or customs of users or operators, and the definitions should be made based on the contents throughout the present specification for describing the present invention.

Taxation  Inhibitor Analysis Device

One aspect of the present invention relates to the analysis of anti-acid tax inhibitor. 1 illustrates an anti-acid tax inhibitor 1000 according to an embodiment of the present invention. Referring to FIG. 1, the anti-acid detergent analysis device 1000 according to the present invention includes a first inlet 1 through which an anti-acid detergent including an amine compound stored in the sample storage unit 201 is introduced, and a decomposition agent storage. A second inlet 2 into which the decomposition agent stored in the unit 202 is introduced, a third inlet 3 into which the sodium hydroxide-sodium thiosulfate (SHST) solution stored in the SHST storage unit 203 is introduced, and a water storage unit A fourth inlet portion 4 is provided, through which water stored in 204 is introduced, and a decomposing agent is introduced from the second inlet portion 2 to the peracid tax inhibitor introduced from the first inlet portion 1 and heated. Disintegrating the anti-acid pickling agent, inducing and distilling water from the third inlet (3) from the third inlet (3) and the SHST solution and the fourth inlet (4) to generate ammonia (NH ₃ ). 1 reaction unit 101; A fifth inlet part 6 through which boric acid stored in the fifth inlet part 5 and the boric acid storage part 205 into which the ammonia distilled from the first reaction part 101 is introduced; A seventh inflow portion 7 into which sulfuric acid stored in the sulfuric acid storage unit 206 flows in, a pH measuring unit 301 measuring internal pH, and a level measuring unit 302 measuring internal level are provided, and the fifth inflow is provided. Collecting ammonia introduced through the portion (5) with boric acid introduced through the sixth inlet (6) to generate a collecting solution, and the sulfuric acid through the seventh inlet (7) to titrate the collecting solution Second reaction unit 102; And a control operation unit electrically connected to the pH measuring unit 301 and the level measuring unit 302 to transmit the measured pH and level data inside the second reaction unit 102 to analyze the concentration of the anti-acid tax inhibitor. 103);

In the present invention, the first reaction unit 101 is provided with a heater (not shown), adds a disintegrating agent to the peroxidation inhibitor, and heats the distillation by adding the SHST solution and water. In addition, although not shown in the drawings, one side of the first reaction unit 101 is provided with a waste gas treatment unit, the unreacted waste gas may be discharged.

Referring to FIG. 1, in one embodiment of the present invention, one side of the first reaction unit 101 and the second reaction unit 102 may include a first discharge unit 21 and a second discharge unit 22, respectively. In addition, the components remaining in the first reaction unit 101 and the second reaction unit 102 may be discharged. For example, it can be discharged using the siphon principle.

Referring to FIG. 1, water stored in the water storage unit 204 may be introduced into the sample storage unit 201 through the eighth inflow unit 8 to dilute the anti-acid tax inhibitor. Since the concentration of the amine compound (HMTA) included in the anti-acid tax inhibitor may be different, the amount of water may be injected such that the amount of water can be diluted 5 times, 10 times, 20 times, 50 times, and 100 times according to the sample injected sample. The optimal concentration can be converted.

In addition, the water stored in the water storage unit 204 is introduced into the second reaction unit 102 through the ninth inlet (9) to adjust the concentration of the collection solution or to wash the inside of the second reaction unit (102). Can be.

In one embodiment, the pH measuring unit 301 measures the pH of the boric acid introduced into the second reaction unit 102 through the sixth inlet 6 in the boric acid storage unit 205, the fifth inflow to the boric acid The sulfuric acid is introduced into the collection solution generated by collecting the ammonia introduced through the unit 5, and the pH of the collection solution may be measured.

The level measuring unit 302 measures the level of boric acid introduced into the second reaction unit 102 through the sixth inlet unit 6 in the boric acid storage unit 205, and the ammonia is collected and collected in the boric acid. The level of the collecting solution and the level of the collecting solution titrated by adding the sulfuric acid can be measured.

The control operation unit 103 may derive the concentration of nitrogen included in the anti-acid tax inhibitor by using the pH data of the pH measuring unit 301 and the level data measured by the level measuring unit 302.

In one embodiment, each of the first to ninth inlets may be provided with a pump, and the pump may be controlled by being electrically connected to the control operation unit 103.

Taxation  Method of analysis of inhibitor

Another aspect of the present invention relates to a method of analyzing the anti-acid tax inhibitor using the apparatus for analyzing the anti-acid tax inhibitor. Figure 2 shows the analysis method of the anti-acid tax inhibitor according to an embodiment of the present invention. Referring to FIG. 2, the analysis method of the anti-acid tax inhibitor is (s101) a step of decomposing the anti-acid tax inhibitor; (s102) ammonia collection step; (s103) collection solution manufacturing step; And (s104) titration step.

More specifically, the method of analyzing the anti-acid detergent comprises (s101) adding a decomposing agent to the anti-acid detergent including the amine compound and heating and decomposing it; (s102) collecting ammonia (NH ₃ ) generated by adding and distilling sodium hydroxide-sodium thiosulfate (SHST) solution and water to the decomposed anti-acid detergent; (s103) collecting the collected ammonia (NH ₃ ) with boric acid to generate a collection solution; And (s104) deriving the nitrogen concentration contained in the ammonia (NH ₃ ) by titrating the collection solution with sulfuric acid.

Hereinafter, a step-by-step description of the analysis method of the anti-acid tax inhibitor according to the present invention.

(s101) Taxation  Inhibitor heating step

The step is to decompose by adding a decomposing agent to the anti-acid detergent including an amine compound and heating. In this step, the anti-acid tax inhibitor and the disintegrating agent react to cause decomposition, oxidation and reduction.

It is required to control the acid concentration of the acid tank which is a direct cause of the acid pickling and peracid tax generated according to the acid concentration used in the pickling process, and an anti-acid tax inhibitor is used to prevent the acid pickling.

In one embodiment of the present invention, an amine compound included in the anti-acid pickling inhibitor can be used a conventional one. For example, it may be hexamethylenetetraamine (HMTA).

In one embodiment, the digestion agent may be prepared by mixing potassium sulfate (K ₂ SO ₄ ), copper sulfate (CuSO ₄ ), sulfuric acid (H ₂ SO ₄ ), and water. In one embodiment the disintegrant is dissolved in 134 g of potassium sulfate (K ₂ SO ₄ ) and 7.3 g of copper sulfate (CuSO ₄ ) in 800 mL of water, then 134 mL of 90% sulfuric acid is added and diluted again with 1 L It can manufacture.

At this time, the potassium sulfate is dissolved in sulfuric acid, thereby increasing the boiling point, and serves to promote decomposition.

The heating temperature may be 350 ℃ ~ 400 ℃. When heating to the above range, while preventing the thermal decomposition of nitrogen contained in the anti-acid detergent, the decomposition of the anti-acid detergent can be easily proceeded. For example, the temperature may be 380 ° C to 400 ° C.

The nitrogen component contained in the anti-acid detergent prevents ammonia (NH ₃ ) from reacting with the decomposing agent, and the ammonia reacts with sulfuric acid (H ₂ SO ₄ ) of the decomposing agent to form ammonium sulfate ((NH ₄ ) ₂ SO ₄ ) is generated.

(s102) ammonia collection step

The step is to collect the ammonia (NH ₃ ) gas generated by adding and distilling sodium hydroxide-sodium thiosulfate (SHST) solution and water to the decomposed anti-acid detergent.

The SHST (sodium hydroxide-sodium thiosulfate, NaOH) solution, sodium hydroxide (sodium hydroxide) and sodium thiosulfate (sodium thiosulfate, Na ₂ S ₂ O ₃ · 5H ₂ 0).

In one embodiment, the SHST solution may be prepared by dissolving 500 g of sodium hydroxide (NaOH) and 25 g of the sodium thiosulfate (Na ₂ S ₂ O ₃ · 5H ₂ 0) in water, and diluting to 1 L by adding water. .

The distillation can be carried out using conventional methods. The distillation may be made at 60 ℃ ~ 100 ℃. The distillation at the temperature may be excellent in collecting the ammonia (NH ₃ ) gas.

(s103) Capture Solution  Manufacturing stage

The step is to collect the collected ammonia (NH ₃ ) with boric acid, to generate a collection solution. When using the boric acid, it is possible to easily collect the ammonia, it may be easy to analyze the amount of nitrogen contained in the anti-acid pickling agent.

(s104) titration step

The step is a step of deriving the nitrogen concentration contained in the ammonia (NH ₃ ) by titrating the collection solution with sulfuric acid. For example, from the amount of sulfuric acid consumed during the titration, the amount of nitrogen contained in the collected ammonia can be calculated.

In one embodiment, the sulfuric acid may use dilute sulfuric acid. For example, sulfuric acid of 0.01 N to 0.05 N (normality) can be used.

In one embodiment, the titration may be performed by measuring the pH of the boric acid, and adding sulfuric acid to the collection solution, adjusting the pH of the collection solution to the pH of the measured boric acid.

When applying the analysis method of the anti-acid tax inhibitor of the present invention, by applying a method of measuring and analyzing the nitrogen contained in the amine, there is an advantage that can be detected even when the sample to be analyzed is present in the acid solution base with a low quantification limit, The anti-acid pickling agent concentration measurement reliability, accuracy and precision is excellent, the anti-pickling of the cold-rolled steel sheet is prevented, and the surface defect prevention effect is excellent, it is possible to improve the work efficiency during the pickling process.

Hereinafter, the configuration and operation of the present invention through the preferred embodiment of the present invention will be described in more detail. However, this is presented as a preferred example of the present invention and in no sense can be construed as limiting the present invention.

Example

The nitrogen concentration of the anti-acid tax inhibitor was analyzed using the anti-acid tax inhibitor as shown in FIG. 1.

5 ml of the anti-acid tax inhibitor sample containing hexamethylenetetraamine (HMTA) stored in the sample storage unit 201 was introduced into the first reaction unit 101 through the first inlet unit 1. At this time, the first discharge part 21 of the first reaction part 101 is closed, and the gas outlet part is discharged through the waste gas treatment part (not shown).

In addition, dissolve 134 g of potassium sulfate (K ₂ SO ₄ ) and 7.3 g of copper sulfate (CuSO ₄ ) in 800 mL of water, then add 134 mL of 90% sulfuric acid, and dilute with 1 L of water to prepare a disintegrant, 500 g of the sodium hydroxide (NaOH) and 25 g of the sodium thiosulfate (Na ₂ S ₂ O ₃ .5H ₂ 0) were dissolved in water, diluted with 1 L of water to prepare a SHST solution.

Subsequently, 5 mL of the disintegrant stored in the disintegrant storage unit 202 was introduced into the first reaction unit 101 through the second inlet unit 2. Thereafter, the heater was operated to cool the inside of the first reaction part 101 to 390 ° C. for 10 minutes, and then cooled for 5 minutes. 5 mL of boric acid stored in the boric acid storage unit 205 was placed in the second reaction unit 102 and the pH of boric acid was measured through the pH measuring unit 301. 30 mL of distilled water stored in the water storage unit 204 is introduced into the first reactor 101 through the fourth inlet unit 4, and the SHST solution stored in the SHST solution storage unit 203 is transferred to the third inlet unit ( 3) through 5mL, and heated to 100 ℃ to evaporate, the generated ammonia (NH ₃ ) is collected through the fifth inlet (5) and introduced into the second reaction unit 102, collected by boric acid Thus, a collecting solution was produced. When the internal level of the second reaction unit 102 measured by the level measuring unit 302 became 20 mL, the heater was stopped.

Then, sulfuric acid stored in the sulfuric acid storage unit 206 was introduced into the collection solution through the seventh inflow unit 7, and the pH of the collection solution was adjusted to the pH of the measured boric acid.

At this time, the pH measuring unit 301 and the level measuring unit 302 measures the pH and level of the appropriate collection solution, the control operation unit 103 electrically connected to the pH measuring unit 301 and the level measuring unit 302 ).

The total nitrogen contained in the anti-acid tax inhibitor by using the pH data of the collection solution measured by the pH measuring unit 301 and the level data of the appropriate collection solution measured by the level measuring unit 302 in the control operation unit 103. The concentration of (TKN) was derived and shown in Table 1 below.

Unit conversion using the results analyzed as in the above Example, converted to the amine compound concentration to derive the result value is shown in Table 1 below.

Figure 3 is a graph comparing the concentration of the amine compound contained in the prepared anti-acid inhibitor and the measured anti-acid detergent. Referring to Table 1 and FIG. 3, the actual data analysis showed an accuracy of 92%, and the precision was measured within 3%, when applying the analysis method using the anti-tax inhibitor analysis device of the present invention, When analyzing the concentration of the amine compound contained in, it was found that the precision and accuracy is excellent.

Simple modifications or changes of the present invention can be easily carried out by those skilled in the art, and all such modifications or changes can be seen to be included in the scope of the present invention.

Claims (5)

1. A first inlet through which an anti-acid tax inhibitor comprising an amine compound is introduced, a second inlet through which a decomposition agent is introduced, a third inlet through which a SHST (sodium hydroxide-sodium thiosulfate) solution is introduced, and a fourth inlet through which water is introduced The deoxidant is added to the anti-acid pickling agent and heated to decompose the anti-acid pickling agent, and the SHST solution and water are introduced into the decomposed anti-acid pickling agent and distilled to generate ammonia (NH ₃ ). 1 reaction part;

   A fifth inlet portion into which the ammonia distilled from the first reaction portion flows in, a sixth inlet portion in which boric acid flows in, a seventh inlet portion in which sulfuric acid flows in, a pH measuring unit measuring internal pH, and a level for measuring internal levels A second reaction part provided with a measurement part and collecting the introduced ammonia with boric acid to generate a collection solution, and titrating the collection solution by introducing the sulfuric acid; And

   And a control calculation unit electrically connected to the pH measuring unit and the level measuring unit to transmit the measured pH and level data inside the second reaction unit to analyze the concentration of the anti-acid tax inhibitor. Analysis device.
2. Adding a disintegrating agent to the peracid-protecting agent including the amine compound and heating the decomposition;

   Collecting ammonia (NH ₃ ) generated by adding a sodium hydroxide-sodium thiosulfate (SHST) solution and water to the decomposed anti-acid detergent;

   Collecting the collected ammonia (NH ₃ ) with boric acid to generate a collection solution; And

   And titrating the collection solution with sulfuric acid to derive the nitrogen concentration contained in the ammonia (NH ₃ ).

   The decomposition agent is a method of analyzing the anti-acid detergent, characterized in that prepared by mixing potassium sulfate (K ₂ SO ₄ ), copper sulfate (CuSO ₄ ), sulfuric acid (H ₂ SO ₄ ) and water.
3. The method of claim 2,

   The heating is an analysis method of the anti-acid detergent, characterized in that at 350 ℃ ~ 400 ℃.
4. The method of claim 2,

   The distillation is a method of analyzing the anti-acid detergent, characterized in that at 65 ℃ ~ 100 ℃.
5. The method of claim 2,

   The titration measures the pH of the boric acid, and

   Adding sulfuric acid to the collection solution, and adjusting the pH of the collection solution to the pH of the measured boric acid.

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