CN111044670B - Cation exchange capacity test method for ammonium type and ammonium type mixed powder ion exchange resin - Google Patents
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Abstract
The invention provides a method for testing the cation exchange capacity of ammonium type and ammonium type mixed powder ion exchange resin, which combines the characteristics of the ammonium type and ammonium type mixed powder ion exchange resin, adopts the conventional distillation and condensation method, adds alkali liquor into the powder resin, and under the condition of heating, active group NH in the powder resin4 +And the ammonium cation exchange capacity in the powder resin is calculated by measuring the concentration of the residual acid in the absorption liquid. The method of the invention not only abandons formaldehyde medicament, but also is simple and easy to operate, and the result is not influenced by dispersant and has good reproducibility.
Description
Technical Field
The invention relates to the technical field of testing of cation exchange capacity of ammonium type powder ion exchange resin, in particular to a method for testing the cation exchange capacity of ammonium type and ammonium type mixed powder ion exchange resin.
Background
The powder ion exchange resin can be widely applied to the fields of condensed water treatment systems in the power industry, water treatment of fuel tanks of nuclear power plants, water treatment of reactors, treatment of radioactive liquid wastes and the like. For example, in a condensed water treatment system of an air cooling unit, powdered resin can be used as a filter medium to be coated on a filter element of a pre-filter so as to achieve the effects of partially desalting and removing suspended solid particles, organic matters and other colloidal substances, and the method has high application value. The conventional physical and chemical properties of the powdered ion exchange resin include water content, particle size, and exchange capacity.
At present, one international method for testing the cation exchange capacity of ammonium type and ammonium type mixed powder resin is the method specified in appendix D of DL/T1138-2009 powdered ion exchange resin for water treatment in thermal power plant, and the testing method is to soak the resin in excessive NaNO3In the solution, after the reaction is finished, the soaking solution is taken and added with 30 percent of formaldehyde solution which is adjusted to be neutral by sodium hydroxide, and then ammonium salt in the soaking solution can react with formaldehyde to generate acid (protonated hexamethylenetetramine and H) with equal mass+) And (4) titrating the acid concentration of the solution after the reaction to calculate the cation exchange capacity.
Due to the volatility and toxicity of formaldehyde, the formaldehyde is harmful to the environment and the body health of testers. In addition, in recent years, in order to make the powder resin have better dispersibility for practical use, various types of dispersants are often added in production, which causes serious disturbance to the measurement of the ammonium cation exchange capacity, and causes variations in the measurement results.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a method for testing the cation exchange capacity of ammonium type and ammonium type mixed powder ion exchange resin, which is simple and easy to operate, has no influence on the test result by a dispersing agent and has good reproducibility.
In order to achieve the purpose, the invention adopts the technical scheme that:
the method for testing the cation exchange capacity of the ammonium type and ammonium type mixed powder ion exchange resin comprises the following steps:
the first step is matched with an experimental device, namely a distillation condensing device, wherein the distillation condensing device comprises a heating sleeve 1, a single-neck round-bottom flask 2 fixed on the heating sleeve 1, a condensing pipe 3 and a ox horn pipe 4 which are sequentially communicated with the outlet of the single-neck round-bottom flask 2, and the tail end of the ox horn pipe 4 extends into an absorption bottle 5;
secondly, preparing 0.9-1.2 mol/L hydrochloric acid standard solution and 0.9-1.2 mol/L sodium hydroxide standard solution, wherein the mass percent of the sodium hydroxide standard solution is 50% of sodium hydroxide aqueous solution; recording the concentration of the hydrochloric acid standard solution as c after calibration 1Concentration of sodium hydroxide Standard solution is c2;
Thirdly, weighing 5-20 g of ammonium or ammonium mixed powder ion exchange resin into a single-mouth round-bottom flask 2, adding 20-30 mL of hydrochloric acid standard solution prepared in the second step and high-purity water into an absorption bottle 5, wherein the adding amount of the high-purity water enables the tail end of the ox horn 4 to be immersed into the solution in the absorption bottle 5, and recording the adding volume V of the hydrochloric acid standard solution1;
Fourthly, quickly adding 10-20 mL of the sodium hydroxide aqueous solution with the mass percentage of 50% and 150-200 mL of high-purity water prepared in the second step into the single-mouth round-bottom flask 2;
fifthly, sealing each interface of the distillation and condensation device, starting heating until the mixture in the single-mouth round-bottom flask 2 boils, then, allowing ammonia and water vapor to escape together, cooling and liquefying the water vapor when the condenser pipe 3 is reached, dissolving most of the ammonia gas in water to form an alkaline condensate, allowing the alkaline condensate to pass through the condenser pipe 3 and enter the absorption bottle 5, allowing the other small part of the ammonia gas which is not dissolved in the water to directly pass through the condenser pipe 3 to the absorption bottle 5 to be absorbed by the acidic absorption liquid and undergo an acid-base neutralization reaction, and continuously heating until 100mL of the condensate enters the absorption bottle 5 to stop the reaction;
sixthly, titrating the solution in the absorption bottle 5 by using the sodium hydroxide standard solution prepared in the second step until the phenolphthalein indicator keeps reddish and keeps for 15s, stopping titration, and recording the volume of the consumed sodium hydroxide standard solution, namely the titration volume of the sodium hydroxide standard solution as V 2;
The wet base cation exchange capacity, Q, is calculated as follows:
in the formula:
c1concentration of hydrochloric acid Standard solution in mol/L;
c2-the concentration of sodium hydroxide standard solution in mol/L;
V1-the addition volume of the hydrochloric acid standard solution in mL;
V2the titration volume of the sodium hydroxide standard solution, in mL;
m is the mass of the ammonium or ammonium mixed powder ion exchange resin and the unit is g.
The invention has the beneficial effects that:
the method combines the characteristics of ammonium type and ammonium type mixed powder ion exchange resin, adopts the conventional distillation and condensation method, and under the heating alkaline condition, active groups NH in the powder resin4 +And the ammonium cation exchange capacity in the powder resin is calculated by measuring the concentration of the residual acid in the absorption liquid. The method of the invention not only abandons formaldehyde medicament, but also is simple and easy to operate, and has good result reproducibility.
Drawings
FIG. 1 is a schematic view of a distillation condensing apparatus.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the following embodiments and the accompanying drawings.
Example 1
The first step of the matching experimental device is a distillation condensing device, as shown in figure 1, the distillation condensing device comprises a heating jacket 1, a single-neck round-bottom flask 2 fixed on the heating jacket 1, a condensing tube 3 and a ox horn tube 4 which are sequentially communicated with the outlet of the single-neck round-bottom flask 2, and the tail end of the ox horn tube 4 extends into an absorption bottle 5.
And preparing 0.9-1.2 mol/L hydrochloric acid standard solution and 0.9-1.2 mol/L sodium hydroxide standard solution, wherein the mass percent of the sodium hydroxide standard solution is 50% of sodium hydroxide aqueous solution. After calibration, the concentration of the hydrochloric acid standard solution is 1.1587mol/L and the concentration of the sodium hydroxide standard solution is 0.9868 mol/L.
In the third step, 10.6922g of the ammonium type mixed powder ion exchange resin (ammonium type/hydrogen oxygen type ═ 1:1) was accurately weighed out in a round-bottom flask as it was, and 25.00mL of the hydrochloric acid standard solution prepared in the second step and 25mL of high purity water were accurately added to an absorption bottle so that the end of the bull horn 4 was immersed in the solution in the absorption bottle 5.
Fourth step to a single neck round bottom flask 2 were rapidly added 15mL of 50% aqueous sodium hydroxide solution and 200mL of highly purified water.
And fifthly, sealing each interface of the distillation and condensation device, starting heating until the mixture in the single-mouth round-bottom flask 2 boils, allowing ammonia and water vapor to escape together, cooling and liquefying the water vapor when the water vapor reaches the condenser pipe 3, dissolving most of the ammonia gas in the water to form alkaline condensate, allowing the alkaline condensate to enter the absorption bottle 5 after passing through the condenser pipe 3, allowing the other small part of the ammonia gas which is not dissolved in the water to directly pass through the condenser pipe 3 to the absorption bottle 5 to be absorbed by the acidic absorption liquid and generate acid-base neutralization reaction, and continuously heating until 100mL of the condensate enters the absorption bottle 5 to stop the reaction.
And sixthly, titrating the solution in the absorption bottle 5 by using a sodium hydroxide standard solution until the phenolphthalein indicator keeps reddish for 15 seconds, stopping titration, and consuming 18.42mL of the sodium hydroxide standard solution.
The wet-based cation exchange capacity Q of the resin was calculated to be 1.01 mmol/L.
Example 2
The first step of the matching experimental device is a distillation condensing device, as shown in figure 1, the distillation condensing device comprises a heating jacket 1, a single-neck round-bottom flask 2 fixed on the heating jacket 1, a condensing tube 3 and a ox horn tube 4 which are sequentially communicated with the outlet of the single-neck round-bottom flask 2, and the tail end of the ox horn tube 4 extends into an absorption bottle 5.
And preparing 0.9-1.2 mol/L hydrochloric acid standard solution and 0.9-1.2 mol/L sodium hydroxide standard solution, wherein the mass percent of the sodium hydroxide standard solution is 50% of sodium hydroxide aqueous solution. After calibration, the concentration of the hydrochloric acid standard solution is 1.1587mol/L and the concentration of the sodium hydroxide standard solution is 0.9868 mol/L.
Third step 5.1078g of mixed powder ion exchange resin of ammonium type (ammonium type/hydrogen oxygen type ═ 1:1) was accurately weighed out in a round-bottomed flask as it was, and 20.00mL of the hydrochloric acid standard solution prepared in the second step and 20mL of high purity water were accurately added to an absorption bottle to immerse the tip of the bull horn 4 in the solution in the absorption bottle 5.
Fourth step to a single neck round bottom flask 2 were rapidly added 10mL of 50% aqueous sodium hydroxide solution and 200mL of highly purified water.
And fifthly, sealing each interface of the distillation and condensation device, starting heating until the mixture in the single-mouth round-bottom flask 2 boils, allowing ammonia and water vapor to escape together, cooling and liquefying the water vapor when the water vapor reaches the condenser pipe 3, dissolving most of the ammonia gas in the water to form alkaline condensate, allowing the alkaline condensate to enter the absorption bottle 5 after passing through the condenser pipe 3, allowing the other small part of the ammonia gas which is not dissolved in the water to directly pass through the condenser pipe 3 to the absorption bottle 5 to be absorbed by the acidic absorption liquid and generate acid-base neutralization reaction, and continuously heating until 100mL of the condensate enters the absorption bottle 5 to stop the reaction. (ii) a
And sixthly, titrating the solution in the absorption bottle by using a sodium hydroxide standard solution until the phenolphthalein indicator keeps reddish for 15 seconds, stopping titration, and consuming 16.80mL of the sodium hydroxide standard solution.
The wet-based cation exchange capacity Q of the resin was calculated to be 1.29 mmol/L.
Example 3
The first step of the matching experimental device is a distillation condensing device, as shown in figure 1, the distillation condensing device comprises a heating jacket 1, a single-neck round-bottom flask 2 fixed on the heating jacket 1, a condensing tube 3 and a ox horn tube 4 which are sequentially communicated with the outlet of the single-neck round-bottom flask 2, and the tail end of the ox horn tube 4 extends into an absorption bottle 5.
And preparing 0.9-1.2 mol/L hydrochloric acid standard solution and 0.9-1.2 mol/L sodium hydroxide standard solution, wherein the mass percent of the sodium hydroxide standard solution is 50% of sodium hydroxide aqueous solution. After calibration, the concentration of the hydrochloric acid standard solution is 1.1587mol/L and the concentration of the sodium hydroxide standard solution is 0.9868 mol/L.
In the third step, 15.1850g of ammonium type mixed powder ion exchange resin (ammonium type/hydrogen oxygen type ═ 2:3) was weighed out accurately in a round-bottomed flask as it was, and 25.00mL of the hydrochloric acid standard solution prepared in the second step and 30mL of highly purified water were added accurately to an absorption flask, so that the end of the bull horn 4 was immersed in the solution in the absorption flask 5.
Fourth step to a single neck round bottom flask 2 were rapidly added 15mL of 50% aqueous sodium hydroxide solution and 200mL of highly purified water.
And fifthly, sealing each interface of the distillation and condensation device, starting heating until the mixture in the single-mouth round-bottom flask 2 boils, allowing ammonia and water vapor to escape together, cooling and liquefying the water vapor when the water vapor reaches the condenser pipe 3, dissolving most of the ammonia gas in the water to form alkaline condensate, allowing the alkaline condensate to enter the absorption bottle 5 after passing through the condenser pipe 3, allowing the other small part of the ammonia gas which is not dissolved in the water to directly pass through the condenser pipe 3 to the absorption bottle 5 to be absorbed by the acidic absorption liquid and generate acid-base neutralization reaction, and continuously heating until 100mL of the condensate enters the absorption bottle 5 to stop the reaction.
And sixthly, titrating the solution in the absorption bottle by using a sodium hydroxide standard solution until the phenolphthalein indicator keeps reddish for 15 seconds, stopping titrating, and consuming 11.00mL of the sodium hydroxide standard solution.
The wet-based cation exchange capacity Q of the resin was calculated to be 1.19 mmol/L.
Example 4
The first step of the matching experimental device is a distillation condensing device, as shown in figure 1, the distillation condensing device comprises a heating jacket 1, a single-neck round-bottom flask 2 fixed on the heating jacket 1, a condensing tube 3 and a ox horn tube 4 which are sequentially communicated with the outlet of the single-neck round-bottom flask 2, and the tail end of the ox horn tube 4 extends into an absorption bottle 5.
And preparing 0.9-1.2 mol/L hydrochloric acid standard solution and 0.9-1.2 mol/L sodium hydroxide standard solution, wherein the mass percent of the sodium hydroxide standard solution is 50% of sodium hydroxide aqueous solution. After calibration, the concentration of the hydrochloric acid standard solution is 1.1587mol/L and the concentration of the sodium hydroxide standard solution is 0.9868 mol/L.
Third step 10.1099g of ammonium type powdery ion exchange resin was accurately weighed in a round-bottomed flask as it was, and 20.00mL of the hydrochloric acid standard solution prepared in the second step and 20mL of high purity water were accurately added to an absorption flask so that the end of a bull horn 4 was immersed in the solution in the absorption flask 5.
Fourth step to a single neck round bottom flask 2 were rapidly added 15mL of 50% aqueous sodium hydroxide solution and 200mL of highly purified water.
And fifthly, sealing each interface of the distillation and condensation device, starting heating until the mixture in the single-mouth round-bottom flask 2 boils, allowing ammonia and water vapor to escape together, cooling and liquefying the water vapor when the water vapor reaches the condenser pipe 3, dissolving most of the ammonia gas in the water to form alkaline condensate, allowing the alkaline condensate to enter the absorption bottle 5 after passing through the condenser pipe 3, allowing the other small part of the ammonia gas which is not dissolved in the water to directly pass through the condenser pipe 3 to the absorption bottle 5 to be absorbed by the acidic absorption liquid and generate acid-base neutralization reaction, and continuously heating until 100mL of the condensate enters the absorption bottle 5 to stop the reaction.
And sixthly, titrating the solution in the absorption bottle by using a sodium hydroxide standard solution until the phenolphthalein indicator keeps reddish for 15s, stopping titrating, and consuming 13.40mL of the sodium hydroxide standard solution.
The wet-based cation exchange capacity Q of the resin was calculated to be 0.98 mmol/L.
Claims (1)
1. The method for testing the cation exchange capacity of the ammonium type and ammonium type mixed powder ion exchange resin is characterized by comprising the following steps: the method comprises the following steps:
the first step is matched with an experimental device, namely a distillation condensing device, wherein the distillation condensing device comprises a heating jacket (1), a single-neck round-bottom flask (2) fixed on the heating jacket (1), a condensing pipe (3) and a ox horn pipe (4) which are sequentially communicated with the outlet of the single-neck round-bottom flask (2), and the tail end of the ox horn pipe (4) extends into an absorption bottle (5);
Preparing 0.9-1.2 mol/L hydrochloric acid standard solution, 0.9-1.2 mol/L sodium hydroxide standard solution and 50% sodium hydroxide aqueous solution in percentage by mass; recording the concentration of the hydrochloric acid standard solution as c after calibration1Concentration of sodium hydroxide Standard solution is c2;
Thirdly, weighing 5-20 g of ammonium or ammonium mixed powder ion exchange resin into a single-mouth round-bottom flask (2), adding 20-30 mL of hydrochloric acid standard solution prepared in the second step and high-purity water into an absorption bottle (5), wherein the adding amount of the high-purity water enables the tail end of a ox horn (4) to be immersed into the solution in the absorption bottle (5), and recording the adding volume V of the hydrochloric acid standard solution1;
Fourthly, quickly adding 10-20 mL of the sodium hydroxide aqueous solution with the mass percentage of 50% and 150-200 mL of high-purity water prepared in the second step into the single-mouth round-bottom flask (2);
fifthly, sealing each interface of the distillation and condensation device, starting heating until a mixture in the single-mouth round-bottom flask (2) boils, wherein ammonia and water vapor escape together, the water vapor is cooled and liquefied when reaching the condenser tube (3), most of ammonia gas is dissolved in water to form alkaline condensate, the alkaline condensate enters the absorption bottle (5) after passing through the condenser tube (3), the other small part of ammonia gas which is not dissolved in water directly passes through the condenser tube (3) to the absorption bottle (5) to be absorbed by the acidic absorption liquid and generate acid-base neutralization reaction, and continuously heating until 100mL of condensate enters the absorption bottle (5) to stop the reaction;
Sixthly, titrating the solution in the absorption bottle (5) by using the sodium hydroxide standard solution prepared in the second step until the phenolphthalein indicator keeps reddish and does not fade for 15s, stopping titration, and recording the volume of the consumed sodium hydroxide standard solution, namely the titration volume of the sodium hydroxide standard solution as V2;
The wet-based cation exchange capacity Q is calculated as follows:
in the formula:
c1-hydrochloric acid standard solution concentration in mol/L;
c2-the concentration of sodium hydroxide standard solution in mol/L;
V1-the addition volume of the hydrochloric acid standard solution in mL;
V2the titration volume of the sodium hydroxide standard solution, in mL;
m is the mass of the ammonium or ammonium mixed powder ion exchange resin and the unit is g.
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CN112268980B (en) * | 2020-10-15 | 2022-03-25 | 西安热工研究院有限公司 | Method for testing lithium type rate of nuclear-grade lithium type cation exchange resin |
CN112285043B (en) * | 2020-10-15 | 2023-04-28 | 西安热工研究院有限公司 | Nuclear grade lithium type cation exchange resin exchange capacity test method |
CN113552283A (en) * | 2021-07-23 | 2021-10-26 | 山东百诺医药股份有限公司 | Method for measuring sulfur trioxide content in sulfur trioxide trimethylamine |
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