CN112920419B - Energy-saving boiler system nano modifier and preparation method thereof - Google Patents
Energy-saving boiler system nano modifier and preparation method thereof Download PDFInfo
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- CN112920419B CN112920419B CN202110124346.2A CN202110124346A CN112920419B CN 112920419 B CN112920419 B CN 112920419B CN 202110124346 A CN202110124346 A CN 202110124346A CN 112920419 B CN112920419 B CN 112920419B
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
- C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
- C02F5/14—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing phosphorus
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Abstract
The invention provides an energy-saving boiler system nano modifier, which is grafted with amino trimethyl phosphine and polyacrylic acidAnd modified Mg-MOF of ethylhexyl palmitate, wherein the preparation raw material of the modified Mg-MOF comprises the following components: 100 parts of Mg-MOF; 5-10 parts of amino trimethyl phosphine idene; 1-3 parts of potassium stearate; 2-5 parts of polyacrylic acid; 3-5 parts of ethylhexyl palmitate; the preparation raw material of the Mg-MOF comprises the following components: 50-80 parts of ethylene diamine tetraacetic acid; mg (magnesium) 3 (C 6 H 5 O 7 ) 2 10-30 parts; 10-20 parts of DMF; 2-5 parts of chloroform; 15-30 parts of absolute ethyl alcohol. The beneficial effects of the invention are as follows: the modifier can effectively prevent the generation of scale in the pipeline or the boiler in the high-pressure steam boiler pipeline, and has higher water stability and thermal stability.
Description
Technical Field
The invention relates to the field of descaling, in particular to an energy-saving boiler system nano modifier and a preparation method thereof.
Background
The steam boiler inevitably has the problems of scale and corrosion after long-time operation, and the main reason for forming the scale in the boiler is that hard components in feed water are continuously evaporated and concentrated at high temperature and high pressure to generate a series of physical and chemical reactions in the boiler, and finally hard and compact scale is formed on a heated surface.
The heat conductivity coefficient of the scale is only one tenth of that of steel, heat transfer is hindered after the heating surface is scaled, and the temperature is increased to keep a certain pressure of the boiler, so that heat loss is caused; and the steel plate and the pipeline are easily burnt due to overheating while the temperature is increased, the overhaul cost is increased, and the service life of the boiler is shortened.
In the prior art, a chemical cleaning agent can be added to disperse and remove the rust and the scale, but the chemical agent is easy to cause secondary damage to the inner wall of the pipeline; in addition, chelating agent and the like can be added to prevent calcium and magnesium ions from crystallizing and precipitating, but the chelating agent in the current market for high-pressure steam boilers is low in efficiency. The high-pressure steam boiler has extremely high requirements on water quality, no treating agent with good effect exists at present, and although water in the pipeline is softened before being injected with water, a large amount of scale still adheres to the pipe wall of the high-pressure steam boiler after the water is not replaced for a long time.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides an energy-saving boiler system nano modifying agent and a preparation method thereof.
An energy-saving boiler system nano modifier comprises modified Mg-MOF grafted with amino trimethyl phosphine, polyacrylic acid and ethylhexyl palmitate, and the preparation raw materials of the modified Mg-MOF comprise the following components:
100 parts of Mg-MOF;
5-10 parts of amino trimethyl phosphine idene;
2-5 parts of polyacrylic acid;
3-5 parts of ethylhexyl palmitate;
the preparation raw material of the Mg-MOF comprises the following components:
50-80 parts of ethylene diamine tetraacetic acid;
Mg 3 (C 6 H 5 O 7 ) 2 10-30 parts;
10-20 parts of DMF;
1-3 parts of potassium stearate;
2-5 parts of chloroform;
15-30 parts of absolute ethyl alcohol.
The preparation method of the energy-saving boiler system nano modifier comprises the following steps:
weighing ethylenediaminetetraacetic acid and Mg according to parts by weight in step (1) 3 (C 6 H 5 O 7 ) 2 DMF, potassium stearate, absolute ethanol and chloroform; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring the mixed solution containing DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring.
And (2) firstly putting the mixed solution prepared in the step (1) into a reaction kettle, setting reaction conditions, slowly adding chloroform until the reaction is finished, obtaining Mg-MOF, and drying the Mg-MOF.
Weighing the Mg-MOF, the amino trimethylene phosphine and the polyacrylic acid prepared in the step (2) according to the mass parts; a mixed solution was prepared by adding weighed aminotrimethylidene phosphine and polyacrylic acid to water, and Mg-MOF was added thereto.
And (4) placing the container filled with the mixed solution prepared in the step (3) into a microwave generator, setting reaction conditions, performing microwave radiation, and performing intermittent microwave radiation.
And (5) weighing ethylhexyl palmitate according to the mass parts, pouring the ethylhexyl palmitate into the container in the step (4), setting reaction conditions, performing microwave radiation by using a microwave generator, and finally drying the modified Mg-MOF.
Preferably, the pH value of the mixed solution in the step (1) is 3-5.
Preferably, the reaction conditions in step (2) are as follows:
the temperature of the reaction kettle is 100-150 ℃, the reaction time is more than or equal to 24 hours, and the reaction kettle is slowly cooled to the room temperature after the reaction is finished.
The mixed solution is subjected to ultrasonic treatment for 1min at the same time interval in the reaction process, and repeated for 2-5 times.
The drying mode is vacuum drying.
Preferably, the reaction conditions in step (4) are as follows:
the frequency of the microwave generator is 915 MHz-2450MHz, the temperature is 80-150 ℃, the processing time is 10min-3h, and in the microwave radiation process, a stirrer is used for continuously stirring the mixed solution, and the rotating speed of the stirrer is 200-1000 r/min.
The intermittent microwave radiation mode is to radiate once every 1min, and the radiation lasts for 2min each time.
Preferably, the reaction conditions in step (5) are as follows:
and (4) pouring ethylhexyl palmitate into the container in the step (4), uniformly stirring, and stopping stirring after uniform stirring.
And (4) adjusting the microwave frequency to be 50HZ-100HZ higher than the microwave frequency in the step (4), adjusting the temperature to be 20-50 ℃ higher than the temperature in the step (4), and adjusting the microwave radiation time to be 10min-1 h.
The drying mode is vacuum drying. .
The invention has the beneficial effects that:
the Mg-MOF material is an organic-inorganic hybrid material with intramolecular pores formed by self-assembly of metal ions through coordination bonds, and the material is characterized in that the material has a metal framework structure, the framework structure has a storage function and can be designed according to needs, but the difficulty of surface grafting groups of the common Mg-MOF is very high due to poor water stability of the common Mg-MOF, and the modified Mg-MOF framework structure has high stability and greatly improved capability of capturing calcium and magnesium ions by grafting amino trimethyl phosphine and polyacrylic acid through the modification method of the invention, so that the generation of scale in a high-pressure steam boiler pipeline can be prevented.
After the surface of the modified Mg-MOF is grafted with the ethylhexyl palmitate, the water stability and the thermal stability of the modified Mg-MOF are obviously improved, and after the ethylhexyl palmitate is grafted, the efficiency of capturing calcium and magnesium ions of the modifying agent is increased, so that the service life and the efficiency of the modifying agent are prolonged.
Drawings
Fig. 1 shows the increase in weight of the 304 stainless steel plate over time.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present solution is explained below by way of specific embodiments.
Example 1:
weighing 50 parts of ethylenediamine tetraacetic acid and Mg in step (1) 3 (C 6 H 5 O 7 ) 2 10 parts of DMF10 parts, 1 part of potassium stearate, 15 parts of absolute ethyl alcohol and 2 parts of chloroform; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring into a mixed solution of DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring; the pH of the mixed solution of DMF, absolute ethanol and water was 3.
And (2) putting the mixed solution prepared in the step (1) into a reaction kettle, wherein the temperature of the reaction kettle is 100 ℃, the mixed solution is reacted in the reaction kettle for 24 hours at an interval of10 hours for ultrasonic treatment for 1min, repeating the ultrasonic treatment for 2 times, slowly cooling the reaction kettle to room temperature after the reaction is finished, continuously and slowly adding chloroform in the whole reaction until the reaction is finished to obtain Mg-MOF, and drying the Mg-MOF in a vacuum drying mode.
Weighing 100 parts of Mg-MOF prepared in the step (2), 5 parts of amino trimethyl phosphine and 2 parts of polyacrylic acid; a mixed solution was prepared by adding weighed aminotrimethylidene phosphine and polyacrylic acid to water, and Mg-MOF was added thereto.
And (4) placing the container filled with the mixed solution prepared in the step (3) in a microwave generator with the frequency of 915 MHz and the temperature of 80 ℃ for microwave radiation for 10min, wherein the microwave radiation is carried out in an intermittent mode, the irradiation is carried out once every 1min, the irradiation lasts for 2min each time, and in the microwave radiation process, a stirrer continuously stirs the mixed solution, and the rotating speed of the stirrer is 200 r/min.
And (5) weighing 3-5 parts of ethylhexyl palmitate, pouring the ethylhexyl palmitate into the container in the step (4), uniformly stirring, stopping stirring after uniform stirring, and performing microwave radiation in a microwave generator with the microwave frequency of 935HZ and the temperature of100 ℃ for 10 min.
And finally, drying the modified Mg-MOF by adopting a vacuum drying oven.
Example 2:
weighing 80 parts of ethylenediamine tetraacetic acid and Mg in step (1) 3 (C 6 H 5 O 7 ) 2 30 parts of DMF20 parts of potassium stearate 3 parts of absolute ethyl alcohol 30 parts of chloroform 5 parts of the mixture; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring into a mixed solution of DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring; the mixed solution of DMF, absolute ethanol and water had a pH of 5.
And (2) putting the mixed solution prepared in the step (1) into a reaction kettle, keeping the temperature of the reaction kettle at 150 ℃, keeping the reaction time in the reaction kettle for 72 hours, carrying out ultrasonic treatment for 1min at intervals of 13 hours, repeating for 5 times, slowly cooling the reaction kettle to room temperature after the reaction is finished, continuously and slowly adding chloroform in the whole reaction until the reaction is finished to obtain Mg-MOF, and drying the Mg-MOF in a vacuum drying mode.
Weighing 100 parts of Mg-MOF prepared in the step (2), 10 parts of amino trimethyl phosphine and 5 parts of polyacrylic acid; a mixed solution was prepared by adding weighed aminotrimethylidene phosphine and polyacrylic acid to water, and Mg-MOF was added thereto.
And (4) placing the container filled with the mixed solution prepared in the step (3) in a microwave generator with the frequency of 2450MHz and the temperature of 150 ℃ for microwave radiation for 3 hours, wherein the microwave radiation is carried out in an intermittent mode, the irradiation is carried out once every 1min, the irradiation lasts for 2min each time, and in the microwave radiation process, a stirrer continuously stirs the mixed solution, and the rotating speed of the stirrer is 1000 r/min.
And (5) weighing 5 parts of ethylhexyl palmitate, pouring the ethylhexyl palmitate into the container in the step (4), uniformly stirring, stopping stirring after uniform stirring, and performing microwave radiation for 1h in a microwave generator with the microwave frequency of 2550HZ and the temperature of 200 ℃.
And finally, drying the modified Mg-MOF by using a vacuum drying oven.
Example 3:
weighing 70 parts of ethylenediamine tetraacetic acid and Mg in the step (1) 3 (C 6 H 5 O 7 ) 2 20 parts of DMF15 parts of potassium stearate 2 parts of absolute ethyl alcohol 20 parts of chloroform 4 parts of the mixture; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring into a mixed solution of DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring; the pH of the mixed solution of DMF, absolute ethanol and water was 4.
And (2) putting the mixed solution prepared in the step (1) into a reaction kettle, wherein the temperature of the reaction kettle is 120 ℃, the reaction in the reaction kettle is carried out for 36 hours, ultrasonic treatment is carried out for 1min at intervals of 8 hours, the ultrasonic treatment is repeated for 4 times, the reaction kettle is slowly cooled to room temperature after the reaction is finished, chloroform is continuously and slowly added into the whole reaction until the reaction is finished, Mg-MOF is obtained, and the Mg-MOF is dried by adopting a vacuum drying mode.
Weighing 100 parts of Mg-MOF prepared in the step (2), 8 parts of amino trimethyl phosphine and 4 parts of polyacrylic acid; a mixed solution was prepared by adding weighed aminotrimethylidene phosphine and polyacrylic acid to water, and Mg-MOF was added thereto.
And (4) placing the container filled with the mixed solution prepared in the step (3) in a microwave generator with the frequency of 2200MHz and the temperature of 120 ℃ for microwave radiation for 1h, wherein the microwave radiation is carried out in an intermittent manner, the irradiation is carried out once every 1min, the irradiation lasts for 2min each time, and in the microwave radiation process, a stirrer continuously stirs the mixed solution, and the rotating speed of the stirrer is 700 r/min.
And (5) weighing 4 parts of ethylhexyl palmitate, pouring the ethylhexyl palmitate into the container in the step (4), uniformly stirring, stopping stirring after uniform stirring, and performing microwave radiation in a microwave generator with the microwave frequency of 2280HZ and the temperature of 160 ℃ for 30 min.
And finally, drying the modified Mg-MOF by adopting a vacuum drying oven.
Comparative example 1:
weighing 70 parts of ethylenediamine tetraacetic acid and Mg in the step (1) 3 (C 6 H 5 O 7 ) 2 20 parts of DMF15 parts, 2 parts of potassium stearate, 20 parts of absolute ethyl alcohol and 4 parts of chloroform; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring into a mixed solution of DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring; the pH of the mixed solution of DMF, absolute ethanol and water was 4.
And (2) putting the mixed solution prepared in the step (1) into a reaction kettle, wherein the temperature of the reaction kettle is 120 ℃, the reaction in the reaction kettle is carried out for 36 hours, ultrasonic treatment is carried out for 1min at intervals of 8 hours, the ultrasonic treatment is repeated for 4 times, the reaction kettle is slowly cooled to room temperature after the reaction is finished, chloroform is continuously and slowly added into the whole reaction until the reaction is finished, Mg-MOF is obtained, and the Mg-MOF is dried by using a vacuum drying oven.
Comparative example 2:
weighing 70 parts of ethylenediamine tetraacetic acid and Mg in the step (1) 3 (C 6 H 5 O 7 ) 2 20 parts of DMF15 parts of potassium stearate 2 parts of absolute ethyl alcohol 20 parts of chloroform 4 parts of the mixture; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring into a mixed solution of DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring; the pH of the mixed solution of DMF, absolute ethanol and water was 4.
And (2) putting the mixed solution prepared in the step (1) into a reaction kettle, wherein the temperature of the reaction kettle is 120 ℃, the reaction in the reaction kettle is carried out for 36 hours, ultrasonic treatment is carried out for 1min at intervals of 8 hours, the ultrasonic treatment is repeated for 4 times, the reaction kettle is slowly cooled to room temperature after the reaction is finished, chloroform is continuously and slowly added into the whole reaction until the reaction is finished, Mg-MOF is obtained, and the Mg-MOF is dried in a vacuum drying mode.
Weighing 100 parts of Mg-MOF prepared in the step (2) and 8 parts of amino trimethylphosphine; a mixed solution was prepared by adding weighed aminotrimethylidene phosphine to water, and Mg-MOF was added thereto.
And (4) placing the container filled with the mixed solution prepared in the step (3) in a microwave generator with the frequency of 2200MHz and the temperature of 120 ℃ for microwave radiation for 1h, wherein the microwave radiation is carried out in an intermittent manner, the irradiation is carried out once every 1min, the irradiation lasts for 2min each time, and in the microwave radiation process, a stirrer continuously stirs the mixed solution, and the rotating speed of the stirrer is 700 r/min.
And finally, drying the modified Mg-MOF by using a vacuum drying oven.
Comparative example 3:
weighing 70 parts of ethylenediamine tetraacetic acid and Mg in the step (1) 3 (C 6 H 5 O 7 ) 2 20 parts of DMF15 parts of potassium stearate 2 parts of absolute ethyl alcohol 20 parts of chloroform 4 parts of the mixture; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring into a mixed solution of DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring; the pH of the mixed solution of DMF, absolute ethanol and water was 4.
And (2) putting the mixed solution prepared in the step (1) into a reaction kettle, wherein the temperature of the reaction kettle is 120 ℃, the reaction in the reaction kettle is carried out for 36 hours, ultrasonic treatment is carried out for 1min at intervals of 8 hours, the ultrasonic treatment is repeated for 4 times, the reaction kettle is slowly cooled to room temperature after the reaction is finished, chloroform is continuously and slowly added into the whole reaction until the reaction is finished, Mg-MOF is obtained, and the Mg-MOF is dried in a vacuum drying mode.
Weighing 100 parts of Mg-MOF and 4 parts of polyacrylic acid prepared in the step (2); a mixed solution was prepared by adding polyacrylic acid to water, and Mg-MOF was added thereto.
And (4) placing the container filled with the mixed solution prepared in the step (3) in a microwave generator with the frequency of 2200MHz and the temperature of 120 ℃ for microwave radiation for 1h, wherein the microwave radiation is carried out in an intermittent manner, the irradiation is carried out once every 1min, the irradiation lasts for 2min each time, and in the microwave radiation process, a stirrer continuously stirs the mixed solution, and the rotating speed of the stirrer is 700 r/min.
And finally, drying the modified Mg-MOF by using a vacuum drying oven.
Comparative example 4:
weighing 70 parts of ethylenediamine tetraacetic acid and Mg in the step (1) 3 (C 6 H 5 O 7 ) 2 20 parts of DMF15 parts of potassium stearate 2 parts of absolute ethyl alcohol 20 parts of chloroform 4 parts of the mixture; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring into a mixed solution of DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring; the pH of the mixed solution of DMF, absolute ethanol and water was 4.
And (2) putting the mixed solution prepared in the step (1) into a reaction kettle, wherein the temperature of the reaction kettle is 120 ℃, the reaction in the reaction kettle is carried out for 36 hours, ultrasonic treatment is carried out for 1min at intervals of 8 hours, the ultrasonic treatment is repeated for 4 times, the reaction kettle is slowly cooled to room temperature after the reaction is finished, chloroform is continuously and slowly added into the whole reaction until the reaction is finished, Mg-MOF is obtained, and the Mg-MOF is dried in a vacuum drying mode.
And (3) weighing 100 parts of Mg-MOF and 4 parts of ethylhexyl palmitate prepared in the step (2), pouring the ethylhexyl palmitate into a container, uniformly stirring, stopping stirring after uniform stirring, and performing microwave radiation for 30min in a microwave generator with the microwave frequency of 2280HZ and the temperature of 160 ℃.
And finally, drying the modified Mg-MOF by using a vacuum drying oven.
Comparative example 5:
weighing 70 parts of ethylenediamine tetraacetic acid and Mg in the step (1) 3 (C 6 H 5 O 7 ) 2 20 parts of DMF15 parts, 2 parts of potassium stearate, 20 parts of absolute ethyl alcohol and 4 parts of chloroform; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring into a mixed solution of DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring; the pH of the mixed solution of DMF, absolute ethanol and water was 4.
And (2) putting the mixed solution prepared in the step (1) into a reaction kettle, wherein the temperature of the reaction kettle is 120 ℃, the reaction in the reaction kettle is carried out for 36 hours, ultrasonic treatment is carried out for 1min at intervals of 8 hours, the ultrasonic treatment is repeated for 4 times, the reaction kettle is slowly cooled to room temperature after the reaction is finished, chloroform is continuously and slowly added into the whole reaction until the reaction is finished, Mg-MOF is obtained, and the Mg-MOF is dried in a vacuum drying mode.
Weighing 100 parts of Mg-MOF prepared in the step (2) and 8 parts of amino trimethylphosphine; a mixed solution was prepared by adding weighed aminotrimethylidene phosphine to water, and Mg-MOF was added thereto.
And (4) placing the container filled with the mixed solution prepared in the step (3) in a microwave generator with the frequency of 2200MHz and the temperature of 120 ℃ for microwave radiation for 1h, wherein the microwave radiation is carried out in an intermittent manner, the irradiation is carried out once every 1min, the irradiation lasts for 2min each time, and in the microwave radiation process, a stirrer continuously stirs the mixed solution, and the rotating speed of the stirrer is 700 r/min.
And (5) weighing 4 parts of ethylhexyl palmitate, pouring the ethylhexyl palmitate into the container in the step (4), uniformly stirring, stopping stirring after uniform stirring, and performing microwave radiation in a microwave generator with the microwave frequency of 2280HZ and the temperature of 160 ℃ for 30 min.
And finally, drying the modified Mg-MOF by using a vacuum drying oven.
Comparative example 6:
weighing 70 parts of ethylenediamine tetraacetic acid and Mg in the step (1) 3 (C 6 H 5 O 7 ) 2 20 parts of DMF15 parts, 2 parts of potassium stearate, 20 parts of absolute ethyl alcohol and 4 parts of chloroform; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring into a mixed solution of DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring; the pH of the mixed solution of DMF, absolute ethanol and water was 4.
And (2) putting the mixed solution prepared in the step (1) into a reaction kettle, wherein the temperature of the reaction kettle is 120 ℃, the reaction in the reaction kettle is carried out for 36 hours, ultrasonic treatment is carried out for 1min at intervals of 8 hours, the ultrasonic treatment is repeated for 4 times, the reaction kettle is slowly cooled to room temperature after the reaction is finished, chloroform is continuously and slowly added into the whole reaction until the reaction is finished, Mg-MOF is obtained, and the Mg-MOF is dried in a vacuum drying mode.
Weighing 100 parts of Mg-MOF and 4 parts of polyacrylic acid prepared in the step (2); adding weighed polyacrylic acid into water, adding Mg-MOF into the prepared solution to prepare a mixed solution, and adding Mg-MOF into the mixed solution.
And (4) placing the container filled with the mixed solution prepared in the step (3) in a microwave generator with the frequency of 2200MHz and the temperature of 120 ℃ for microwave radiation for 1h, wherein the microwave radiation is carried out in an intermittent manner, the irradiation is carried out once every 1min, the irradiation lasts for 2min each time, and in the microwave radiation process, a stirrer continuously stirs the mixed solution, and the rotating speed of the stirrer is 700 r/min.
And (5) weighing 4 parts of ethylhexyl palmitate, pouring the ethylhexyl palmitate into the container in the step (4), uniformly stirring, stopping stirring after uniform stirring, and performing microwave radiation in a microwave generator with the microwave frequency of 2280HZ and the temperature of 160 ℃ for 30min again.
And finally, drying the modified Mg-MOF by adopting a vacuum drying oven.
Comparative example 7:
weighing 70 parts of ethylenediamine tetraacetic acid and Mg in the step (1) 3 (C 6 H 5 O 7 ) 2 20 parts of DMF15 parts of potassium stearate 2 parts of absolute ethyl alcohol 20 parts of chloroform 4 parts of the mixture; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring into a mixed solution of DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring; the pH of the mixed solution of DMF, absolute ethanol and water was 4.
And (2) putting the mixed solution prepared in the step (1) into a reaction kettle, wherein the temperature of the reaction kettle is 120 ℃, the reaction in the reaction kettle is carried out for 36 hours, ultrasonic treatment is carried out for 1min at intervals of 8 hours, the ultrasonic treatment is repeated for 4 times, the reaction kettle is slowly cooled to room temperature after the reaction is finished, chloroform is continuously and slowly added into the whole reaction until the reaction is finished, Mg-MOF is obtained, and the Mg-MOF is dried by adopting a vacuum drying mode.
Weighing 100 parts of Mg-MOF prepared in the step (2), 8 parts of amino trimethyl phosphine and 4 parts of polyacrylic acid; a mixed solution was prepared by adding weighed aminotrimethylidene phosphine and polyacrylic acid to water, and Mg-MOF was added thereto.
And (4) placing the container filled with the mixed solution prepared in the step (3) in a microwave generator with the frequency of 2200MHz and the temperature of 120 ℃ for microwave radiation for 1h, wherein the microwave radiation is carried out in an intermittent manner, the irradiation is carried out once every 1min, the irradiation lasts for 2min each time, and in the microwave radiation process, a stirrer continuously stirs the mixed solution, and the rotating speed of the stirrer is 700 r/min.
And finally, drying the modified Mg-MOF by using a vacuum drying oven.
Comparative example 8:
weighing 70 parts of ethylenediamine tetraacetic acid and Mg in the step (1) 3 (C 6 H 5 O 7 ) 2 20 parts of DMF15 parts, 20 parts of absolute ethyl alcohol and 4 parts of chloroform; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring into a mixed solution of DMF, absolute ethyl alcohol and water, and uniformly stirring; the pH of the mixed solution of DMF, absolute ethanol and water was 4.
And (2) putting the mixed solution prepared in the step (1) into a reaction kettle, wherein the temperature of the reaction kettle is 120 ℃, the reaction in the reaction kettle is carried out for 36 hours, ultrasonic treatment is carried out for 1min at intervals of 8 hours, the ultrasonic treatment is repeated for 4 times, the reaction kettle is slowly cooled to room temperature after the reaction is finished, chloroform is continuously and slowly added into the whole reaction until the reaction is finished, Mg-MOF is obtained, and the Mg-MOF is dried in a vacuum drying mode.
Weighing 100 parts of Mg-MOF prepared in the step (2), 8 parts of amino trimethyl phosphine and 4 parts of polyacrylic acid; a mixed solution was prepared by adding weighed aminotrimethylidene phosphine and polyacrylic acid to water, and Mg-MOF was added thereto.
And (4) placing the container filled with the mixed solution prepared in the step (3) in a microwave generator with the frequency of 2200MHz and the temperature of 120 ℃ for microwave radiation for 1h, wherein the microwave radiation is carried out in an intermittent manner, the irradiation is carried out once every 1min, the irradiation lasts for 2min each time, and in the microwave radiation process, a stirrer continuously stirs the mixed solution, and the rotating speed of the stirrer is 700 r/min.
And (5) weighing 4 parts of ethylhexyl palmitate, pouring the ethylhexyl palmitate into the container in the step (4), uniformly stirring, stopping stirring after uniform stirring, and performing microwave radiation in a microwave generator with the microwave frequency of 2280HZ and the temperature of 160 ℃ for 30 min.
And finally, drying the modified Mg-MOF by using a vacuum drying oven.
The modified Mg-MOF prepared in examples 1-3 and comparative examples 1-8 were tested, and the specific results are as follows:
pouring a proper amount of tap water into a pressure vessel with the temperature of 80 ℃ and the pressure of 2MPa, adding the intervention agent prepared in the examples 1-3 and 1-8 into the tap water according to 0.5g/L, uniformly stirring, finally soaking three pieces of 304 stainless steel in the pressure vessel, simultaneously taking out the 304 stainless steel plates after a certain time, and respectively testing the weight increase of the stainless steel plates and the hardness of water quality by using a balance and hardness tester.
As can be seen from tables 1 and 2, example 3 is the best example, and the rate of scale formation of the stainless steel plate after the modifier prepared in example 3 is added is very slow, and is reduced by about 92% compared with the scale formation amount of the blank experiment.
The amount of scale formation was substantially unchanged after addition of the modifier prepared in comparative example 1; the structural amount is reduced after the modifier prepared in the comparative examples 2 and 3 is added, but the difference of the modifier compared with the comparative example 3 is large, which shows that the modifier and the polyacrylic acid play a synergistic role after the amino trimethyl idene phosphine and the polyacrylic acid are grafted; example 8, potassium stearate is not added when Mg-MOF is prepared, compared with example 3, the scale inhibition effect of the steel plate is very poor, and the framework structure of the Mg-MOF is unstable; comparative example 5 and comparative example 6 compared with comparative example 2 and comparative example 3, respectively, comparative example 5 and comparative example 6 showed better scale inhibition effect, and comparative example 7 compared with example 3, comparative example 7 was slightly inferior, indicating that grafted ethylhexyl palmitate could increase the scale removal efficiency of the modifier.
The hardness values of the water in the pressure vessel in table 2 are also substantially proportional to the amount of fouling of the examples and comparative examples.
TABLE 1304 weight change added to stainless Steel plate
TABLE 2 hardness change of water in pressure vessel
Claims (5)
1. The energy-saving boiler system nano modifying agent is characterized in that: the modifier is modified Mg-MOF grafted with amino trimethyl phosphine, polyacrylic acid and ethylhexyl palmitate, and the preparation raw materials of the modified Mg-MOF comprise the following components:
100 parts of Mg-MOF;
5-10 parts of amino trimethyl phosphine idene;
2-5 parts of polyacrylic acid;
3-5 parts of ethylhexyl palmitate;
the preparation raw material of the Mg-MOF comprises the following components:
50-80 parts of ethylene diamine tetraacetic acid;
Mg 3 (C 6 H 5 O 7 ) 2 10-30 parts;
10-20 parts of DMF;
1-3 parts of potassium stearate;
2-5 parts of chloroform;
15-30 parts of absolute ethyl alcohol;
the preparation method of the energy-saving boiler system nano modifier is characterized by comprising the following steps:
weighing ethylenediaminetetraacetic acid and Mg according to parts by weight in step (1) 3 (C 6 H 5 O 7 ) 2 DMF, potassium stearate, chloroform and absolute ethanol; weighing ethylenediaminetetraacetic acid and Mg 3 (C 6 H 5 O 7 ) 2 Pouring the mixture solution containing DMF, potassium stearate, absolute ethyl alcohol and water, and uniformly stirring;
step (2) firstly putting the mixed solution prepared in the step (1) into a reaction kettle, setting reaction conditions, slowly adding chloroform until the reaction is finished to obtain Mg-MOF, and drying the Mg-MOF;
weighing Mg-MOF, amino trimethylphosphine and polyacrylic acid prepared in the step (2) according to the mass parts; adding weighed amino trimethyl phosphine and polyacrylic acid into water to prepare a mixed solution, and adding Mg-MOF into the mixed solution;
step (4) placing the container filled with the mixed solution prepared in the step (3) into a microwave generator, setting reaction conditions, performing microwave radiation, and performing intermittent microwave radiation;
and (5) weighing ethylhexyl palmitate according to the mass parts, pouring the ethylhexyl palmitate into the container in the step (4), setting reaction conditions, performing microwave radiation by using a microwave generator, and finally drying the modified Mg-MOF.
2. The energy-saving boiler system nano improver according to claim 1, wherein in the step (1), the pH value of the mixed solution is 3-5.
3. The energy-saving boiler system nano modifier according to claim 1, wherein in the step (2), the reaction conditions are as follows:
the temperature of the reaction kettle is 100-150 ℃, the reaction time is more than or equal to 24 hours, and the reaction kettle is slowly cooled to the room temperature after the reaction is finished;
carrying out ultrasonic treatment on the mixed solution for 1min at the same time interval in the reaction process, and repeating for 2-5 times;
the drying mode is vacuum drying.
4. The energy-saving boiler system nano modifier according to claim 1, wherein in the step (4), the reaction conditions are as follows:
the frequency of the microwave generator is 915 MHz-2450MHz, the temperature of the microwave generator is 80-150 ℃, the processing time of the microwave generator is 10min-3h, and in the microwave radiation process, a stirrer is used for continuously stirring the mixed solution, and the rotating speed of the stirrer is 200-1000 r/min;
the intermittent microwave radiation mode is microwave radiation once every 1min, and the radiation lasts for 2min each time.
5. The energy-saving boiler system nano modifier according to claim 1, wherein in the step (5), the reaction conditions are as follows:
pouring ethylhexyl palmitate into the container in the step (4), uniformly stirring, and stopping stirring after uniformly stirring;
adjusting the microwave frequency to be 50HZ-100HZ higher than the microwave frequency in the step (4), adjusting the temperature to be 20-50 ℃ higher than the temperature in the step (4), and adjusting the microwave radiation time to be 10min-1 h;
the drying mode is vacuum drying.
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| JPS5881494A (en) * | 1981-11-11 | 1983-05-16 | Toagosei Chem Ind Co Ltd | Composition for water purifying agent |
| BR9503967A (en) * | 1994-09-12 | 1996-09-24 | Rohm & Haas | Process of inhibiting scale formation |
| DE102005010855A1 (en) * | 2005-03-10 | 2006-09-14 | Lanxess Deutschland Gmbh | Aqueous conditioning agent, useful as a pelleting agent, comprises polysuccinimide or its partial hydrolysate in combination with fatty acid amides |
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