CN113430030A - Decoking agent for boiler - Google Patents
Decoking agent for boiler Download PDFInfo
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- CN113430030A CN113430030A CN202110837780.5A CN202110837780A CN113430030A CN 113430030 A CN113430030 A CN 113430030A CN 202110837780 A CN202110837780 A CN 202110837780A CN 113430030 A CN113430030 A CN 113430030A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L10/00—Use of additives to fuels or fires for particular purposes
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Abstract
The invention discloses a decoking agent for a boiler, which comprises 50-80% of nitrate mixture, 10-40% of polymer microspheres and 1-10% of dispersing agent by mass. According to the invention, the hydrophilic polyethylene glycol chain segment and the lipophilic organic silicon chain segment are combined together to form the macromolecular polymer as the dispersing agent, so that the decoking agent can be dispersed more uniformly in the decoking process, and a better decoking effect can be achieved. In addition, the decoking agent also uses polymer microspheres, and after the decoking agent is dispersed and heated under the action of the dispersing agent, substances in the microspheres expand in volume and finally break through the outer layer to release gas, so that the coke layer is broken, the coke layer is changed from a compact structure to a loose structure, and the decoking rate is obviously improved.
Description
Technical Field
The invention relates to the field of decoking agents, in particular to a decoking agent for a boiler.
Background
At present, most of power generation facilities in China still use a coal burning method and can last for a long time. In the existing coal-fired method, coking is a common problem in the operation of a coal-fired boiler. The ash in the fuel is mostly melted to a liquid state or in a softened state at high temperature. The closer to the waterwall the lower the temperature, the further outward from the center of the combustion flame, due to the heat absorption of the waterwall. Under normal conditions, ash will change from a liquid to a softened and thus solid state as the temperature decreases. If the ash still remains softened and encounters the heated surface, it cools and adheres to the heated surface, forming coke. The boiler coking of large-scale unit power plant is more serious, often needs to carry out artifical decoking in the operation process, still need to shut down the stove and carry out artifical coking when the coking is serious, seriously influences coal fired power plant's safe operation, has increased workman's intensity of labour, and decoking work also has very big potential safety hazard simultaneously.
Therefore, more and more companies have studied decoking agents, for example, patent application with publication number CN109679704A discloses a decoking agent and a preparation method thereof, which can lower the combustion temperature by adding copper ions, make the combustion more sufficient, and delay the time of coking, but inevitably generate coking, and then still need to be shut down for manual decoking. In the prior art, a method for adding peroxide into a decoking agent is also available, so that oxygen and oxide are generated after decomposition of the decoking agent, and the decoking agent is combusted more fully.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the above problems, an object of the present invention is to provide a decoking agent for a high boiler, which has excellent dispersibility.
The technical scheme of the invention is as follows:
a decoking agent for a boiler comprises the following components in percentage by mass: 50-80% of nitrate mixture, 10-40% of polymer microspheres and 1-10% of dispersing agent.
As a further aspect of the present invention, the nitrate mixture used in the present invention is a mixture comprising magnesium nitrate, copper nitrate and nickel nitrate; specifically, the nitrate mixture mainly comprises copper nitrate and magnesium nitrate, and the mass ratio of the magnesium nitrate to the copper nitrate to the nickel nitrate is 1:1-1.2: 0.1-0.4.
In a further embodiment of the present invention, the dispersant used in the present invention is a polymeric dispersant and is an amphiphilic block copolymer.
As a further aspect of the present invention, the structure of the dispersant used in the present invention is as follows:
wherein x represents an integer of 5-20, y represents an integer of 15-50, z represents an integer of 10-30, and n represents an integer of 100-300.
As a further aspect of the present invention, the method for preparing the dispersant comprises the steps of:
(1) respectively carrying out vacuum dehydration on the unit alcohol, the hydroxyl silicone oil and the polyethylene glycol at the temperature of 100-130 ℃, and controlling the moisture content to be less than 0.05 percent;
(2) adding the raw materials and Toluene Diisocyanate (TDI) into a reactor, and reacting at 50-80 ℃ until the NCO value is less than 0.03%;
(3) adding succinic anhydride into a reactor, and reacting at 50-80 ℃ until the acid value is less than 10 mgKOH/g;
(4) adding linear polyethyleneimine into a reactor, reacting at the temperature of 100-150 ℃, and simultaneously vacuumizing to remove generated water until the acid value is less than 3 mgKOH/g;
(5) and discharging, cooling and grinding at low temperature into particles to obtain the dispersing agent.
In a further embodiment of the present invention, in the above preparation method, the molar ratio of monoalcohol, hydroxy silicone oil, polyethylene glycol, toluene diisocyanate, succinic anhydride and linear polyethyleneimine is 0.2-0.5:1:1-1.2:1.5-2.5:1-1.2: 0.0001-0.0005.
As a further scheme of the invention, the polymer microspheres used in the invention have an irregular spherical structure consisting of an outer layer and a core layer and have the characteristics of expansion with heat and contraction with cold. Specifically, the outer layer is a polymer outer layer formed by free radical polymerization, the inner layer is hexadecane, and the hexadecane can be changed into gas from liquid when being heated, so that the whole microspheres expand in volume, finally the gas is released, the coke layer is damaged, the coke layer is changed into a loose structure from a compact structure, and the subsequent decoking work is facilitated.
As a further aspect of the present invention, the method for preparing the polymeric microspheres used in the present invention comprises the steps of:
(1) adding polymerizable monomer containing carbon-carbon double bond, hexadecyl alkane, emulsifier and water into a container, and emulsifying at the rotating speed of 5000-10000 r/min;
(2) respectively putting a photoinitiator and the emulsified liquid prepared in the step (1) into a reactor, and carrying out polymerization reaction at 60-80 ℃;
(3) and after the polymerization is finished, performing centrifugal filtration to obtain the polymer microspheres.
Specifically, the mass ratio of the polymerizable monomer containing carbon-carbon double bonds, the hexadecane and the emulsifier is 20-60:40-80: 1-5; the polymerizable monomer containing double bonds is selected from one or a mixture of more of styrene, methyl styrene, acrylic acid, methacrylic acid, acrylonitrile, glycidyl methacrylate, methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl methacrylate, butyl acrylate, butyl methacrylate, isobornyl methacrylate, vinyl pyrrolidone, vinyl caprolactam, allyl methacrylate and phenyl methacrylate.
Specifically, the emulsifier is one or more selected from sodium dodecyl benzene sulfonate, polyoxyethylene nonyl phenyl ether and sodium vinyl sulfonate.
Specifically, the particle size of the microsphere obtained by the preparation method is 20-200 μm.
As a further scheme of the invention, the particle size of the boiler decoking agent prepared by the method is 100-300 meshes.
The technical scheme provided by the invention has the beneficial effects that:
according to the invention, the hydrophilic polyethylene glycol chain segment and the lipophilic organic silicon chain segment are combined together to form the macromolecular polymer as the dispersing agent, so that the decoking agent can be dispersed more uniformly in the decoking process, and a better decoking effect can be achieved. In addition, the decoking agent also uses polymer microspheres, and after the decoking agent is dispersed and heated under the action of the dispersing agent, substances in the microspheres expand in volume and finally break through the outer layer to release gas, so that the coke layer is broken, the coke layer is changed from a compact structure to a loose structure, and the decoking rate is obviously improved.
Detailed description of the invention
The present invention will be further described below by way of specific examples.
In the following examples, those whose operations are not subject to the conditions indicated, are carried out according to the conventional conditions or conditions recommended by the manufacturer. In the scheme of the invention, the hydroxyl silicone oil is purchased from Dow Corning, the polyethylene glycol is purchased from Dow Town Lanzhou, the linear polyethyleneimine is purchased from Japan catalyst Co., Ltd, and other used raw materials are purchased from national medicine reagents and an avadin reagent.
Dispersant synthesis example 1:
respectively carrying out vacuum dehydration on 18.6g of dodecanol, 100g of hydroxy silicone oil with average molecular weight of 1000g/mol and 100g of polyethylene glycol with average molecular weight of 1000g/mol at the temperature of 105 ℃, and controlling the moisture content to be less than 0.05%;
adding the raw materials and 34.8g of Toluene Diisocyanate (TDI) into a reactor, and reacting at 70 ℃ until the NCO value is less than 0.03%;
adding 10g of succinic anhydride into a reactor, and reacting at 80 ℃ until the acid value is less than 10 mgKOH/g;
adding 4.3g of linear polyethyleneimine with the average molecular weight of 10000g/mol into a reactor, reacting at 135 ℃, and simultaneously vacuumizing to remove generated water until the acid value is less than 3 mgKOH/g;
and (3) discharging, cooling, grinding at low temperature to obtain particles to obtain the dispersing agent 1.
Dispersant Synthesis example 2
Respectively carrying out vacuum dehydration on 18.6g of dodecanol, 100g of hydroxy silicone oil with average molecular weight of 1000g/mol and 100g of polyethylene glycol with average molecular weight of 1000g/mol at the temperature of 105 ℃, and controlling the moisture content to be less than 0.05%;
adding the raw materials and 34.8g of Toluene Diisocyanate (TDI) into a reactor, and reacting at 70 ℃ until the NCO value is less than 0.03%;
adding 10g of succinic anhydride into a reactor, and reacting at 80 ℃ until the acid value is less than 10 mgKOH/g;
adding 4.3g of linear polyethyleneimine with the average molecular weight of 25000g/mol into a reactor, reacting at 135 ℃, and simultaneously vacuumizing to remove generated water until the acid value is less than 3 mgKOH/g;
and (4) discharging, cooling, grinding at low temperature to obtain particles to obtain the dispersing agent 2.
Dispersant Synthesis example 3
Respectively carrying out vacuum dehydration on 12g of hexadecanol, 200g of hydroxy silicone oil with average molecular weight of 2000g/mol and 100g of polyethylene glycol with average molecular weight of 1000g/mol at the temperature of 105 ℃, and controlling the water content to be less than 0.05%;
adding the raw materials and 17.4g of Toluene Diisocyanate (TDI) into a reactor, and reacting at 70 ℃ until the NCO value is less than 0.03%;
adding 5g of succinic anhydride into a reactor, and reacting at 80 ℃ until the acid value is less than 10 mgKOH/g;
adding 2.5g of linear polyethyleneimine with the average molecular weight of 25000g/mol into a reactor, reacting at 135 ℃, and simultaneously vacuumizing to remove generated water until the acid value is less than 3 mgKOH/g;
and cooling to low temperature after discharging, and grinding into particles to obtain the dispersing agent 3.
Dispersant Synthesis example 4
Respectively carrying out vacuum dehydration on 12g of hexadecanol, 100g of hydroxyl silicone oil with average molecular weight of 1000g/mol and 200g of polyethylene glycol with average molecular weight of 2000g/mol at the temperature of 105 ℃, and controlling the water content to be less than 0.05%;
adding the raw materials and 17.4g of Toluene Diisocyanate (TDI) into a reactor, and reacting at 70 ℃ until the NCO value is less than 0.03%;
adding 5g of succinic anhydride into a reactor, and reacting at 80 ℃ until the acid value is less than 10 mgKOH/g;
adding 2.5g of linear polyethyleneimine with the average molecular weight of 25000g/mol into a reactor, reacting at 135 ℃, and simultaneously vacuumizing to remove generated water until the acid value is less than 3 mgKOH/g;
and (4) discharging, cooling, grinding at low temperature to obtain particles to obtain the dispersing agent 4.
Dispersant comparative example 1
Respectively carrying out vacuum dehydration on 12g of hexadecanol and 200g of hydroxyl silicone oil with average molecular weight of 1000g/mol at the temperature of 105 ℃, wherein the final water content is less than 0.05%;
adding the raw materials and 17.4g of Toluene Diisocyanate (TDI) into a reactor, and reacting at 70 ℃ until the NCO value is less than 0.03%;
adding 5g of succinic anhydride into a reactor, and reacting at 80 ℃ until the acid value is less than 10 mgKOH/g;
adding 2.5g of linear polyethyleneimine with the average molecular weight of 25000g/mol into a reactor, reacting at 135 ℃, and simultaneously vacuumizing to remove generated water until the acid value is less than 3 mgKOH/g;
and cooling to low temperature after discharging, and grinding into particles to obtain the comparative dispersant 1.
Dispersant comparative example 2
Respectively carrying out vacuum dehydration on 12g of hexadecanol and 200g of polyethylene glycol with the average molecular weight of 1000g/mol at the temperature of 105 ℃, wherein the final water content is less than 0.05%;
adding the raw materials and 17.4g of Toluene Diisocyanate (TDI) into a reactor, and reacting at 70 ℃ until the NCO value is less than 0.03%;
adding 5g of succinic anhydride into a reactor, and reacting at 80 ℃ until the acid value is less than 10 mgKOH/g;
adding 2.5g of linear polyethyleneimine with the average molecular weight of 25000g/mol into a reactor, reacting at 135 ℃, and simultaneously vacuumizing to remove generated water until the acid value is less than 3 mgKOH/g;
and cooling to low temperature after discharging, and grinding into particles to obtain the comparative dispersant 2.
Polymer microsphere synthesis example 1:
adding 10g of styrene, 20g of butyl acrylate, 20g of vinyl pyrrolidone, 50g of hexadecane, 2g of sodium dodecyl benzene sulfonate serving as an emulsifier and 100g of water into a container, and emulsifying at the rotating speed of 10000 r/min;
2g of initiator potassium persulfate was dissolved in 100g of water, and the resulting solution and the above emulsified liquid were put into a reactor, respectively, to carry out polymerization at 80 ℃;
after the polymerization is finished, the microspheres can form precipitates to be separated from the aqueous solution, and the polymer microspheres 1 are obtained after centrifugal filtration.
Polymer microsphere synthesis example 2:
adding 5g of methacrylic acid, 10g of butyl acrylate, 5g of isobornyl methacrylate, 10g of allyl methacrylate, 70g of hexadecane, 2g of emulsifier sodium vinylsulfonate and 100g of water into a container, and emulsifying at the rotating speed of 10000 r/min;
2g of initiator potassium persulfate was dissolved in 100g of water, and the resulting solution and the above emulsified liquid were put into a reactor, respectively, to carry out polymerization at 80 ℃;
after the polymerization is finished, the microspheres can form precipitates to be separated from the aqueous solution, and the polymer microspheres 2 are obtained after centrifugal filtration.
Polymer microsphere synthesis example 3:
adding 5g of methacrylic acid, 5g of phenyl methacrylate, 5g of isobornyl methacrylate, 5g of vinyl pyrrolidone, 80g of hexadecane, 2g of emulsifier sodium vinyl sulfonate and 100g of water into a container, and emulsifying at the rotating speed of 10000 r/min;
2g of initiator potassium persulfate was dissolved in 100g of water, and the resulting solution and the above emulsified liquid were put into a reactor, respectively, to carry out polymerization at 80 ℃;
after the polymerization is finished, the microspheres can form precipitates to be separated from the aqueous solution, and the polymer microspheres 3 are obtained after centrifugal filtration.
Polymer microsphere synthesis example 4:
adding 10g of methacrylic acid, 20g of allyl methacrylate, 20g of isobornyl methacrylate, 10g of vinyl caprolactam, 40g of hexadecane, 2g of emulsifier nonylphenol polyoxyethylene ether and 100g of water into a container, and emulsifying at the rotating speed of 10000 r/min;
2g of initiator potassium persulfate was dissolved in 100g of water, and the resulting solution and the above emulsified liquid were put into a reactor, respectively, to carry out polymerization at 80 ℃;
after the polymerization is finished, the microspheres can form precipitates to be separated from the aqueous solution, and the polymer microspheres 4 are obtained after centrifugal filtration.
Polymeric microspheres comparative example 1:
adding 25g of methacrylic acid, 25g of phenyl methacrylate, 25g of isobornyl methacrylate, 25g of vinyl pyrrolidone, 2g of sodium vinyl sulfonate as an emulsifier and 100g of water into a container, and emulsifying at the rotating speed of 10000 r/min;
2g of initiator potassium persulfate was dissolved in 100g of water, and the resulting solution and the above emulsified liquid were put into a reactor, respectively, to carry out polymerization at 80 ℃;
after polymerization, the microspheres can form precipitates to be separated from the aqueous solution, and the microspheres are obtained by centrifugal filtration, so that the comparative polymer microspheres 1 are obtained.
Dispersibility test sample 1:
40g of magnesium nitrate, 40g of copper nitrate, 5g of nickel nitrate and 5g of dispersant 1 were mixed by a high-speed mixer to prepare a homogeneous system.
Dispersibility test sample 2:
40g of magnesium nitrate, 40g of copper nitrate, 5g of nickel nitrate and 5g of dispersant 2 were mixed by a high-speed mixer to prepare a homogeneous system.
Dispersibility test sample 3:
40g of magnesium nitrate, 40g of copper nitrate, 5g of nickel nitrate and 5g of dispersant 3 were mixed by a high-speed mixer to prepare a homogeneous system.
Dispersibility test sample 4:
40g of magnesium nitrate, 40g of copper nitrate, 5g of nickel nitrate and 5g of dispersant 4 were mixed by a high-speed mixer to prepare a homogeneous system.
Dispersibility test sample 5:
40g of magnesium nitrate, 40g of copper nitrate, 5g of nickel nitrate and 5g of comparative dispersant 1 were mixed by a high-speed mixer to prepare a homogeneous system.
Dispersibility test sample 6:
40g of magnesium nitrate, 40g of copper nitrate, 5g of nickel nitrate and 5g of comparative dispersant 2 were mixed by a high-speed mixer into a homogeneous system.
Dispersibility test sample 7:
40g of magnesium nitrate, 40g of copper nitrate and 5g of nickel nitrate were mixed by a high-speed mixer to prepare a homogeneous system.
Example 1
30g of magnesium nitrate, 30g of copper nitrate, 10g of nickel nitrate, 25g of polymeric microspheres 1 and 5g of dispersing agent 1 were mixed by a high-speed mixer to form a uniform system.
Example 2
30g of magnesium nitrate, 30g of copper nitrate, 10g of nickel nitrate, 25g of polymeric microspheres 2 and 5g of dispersing agent 1 were mixed by a high-speed mixer to form a uniform system.
Example 3
30g of magnesium nitrate, 30g of copper nitrate, 10g of nickel nitrate, 25g of polymeric microspheres 3 and 5g of dispersing agent 1 were mixed by a high-speed mixer to form a uniform system.
Example 4
30g of magnesium nitrate, 30g of copper nitrate, 10g of nickel nitrate, 25g of polymeric microspheres 4 and 5g of dispersing agent 1 were mixed by a high-speed mixer to form a uniform system.
Comparative example 1
30g of magnesium nitrate, 30g of copper nitrate, 10g of nickel nitrate, 25g of comparative polymer microspheres 1, 5g of dispersant 1 were mixed by a high speed mixer into a homogeneous system.
And (3) testing the dispersibility:
the same amount of the above-prepared dispersibility test samples 1 to 7 were taken and added to the boiler, 10 point samples were taken after 1 hour of operation, the nickel content (unit is ppm) in the 10 samples was measured by ICP and the dispersion thereof was calculated, the smaller the dispersion, the better the dispersion effect, and the results are shown in table 1 below.
TABLE 1
From the data in the table, the dispersant used in the invention has better dispersion performance, and can better disperse the decoking agent in the boiler, thereby achieving more comprehensive decoking effect.
Evaluation of decoking Performance:
the ash removal and decoking rates of the decoking agents prepared in examples 1 to 4 and comparative example 1 were respectively tested. The test method comprises the following steps: firstly, measuring the weight of a boiler W1, roasting the boiler at 1200 ℃ for 1 hour, measuring the weight of the boiler to be W2, spraying the same amount of the decoking agent prepared in the examples 1 to 4 and the comparative example 1 on the boiler, standing the boiler at room temperature for 2 hours, rinsing the boiler with sponge under the flow of hot water, and drying the boiler to obtain W3; ash removal and coke removal rate { (W2-W3)/(W2-W1) } 100%, the results are shown in table 2 below:
TABLE 2
Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | |
Ash and coke removing rate | 98.9% | 99.3% | 99.5% | 97.8% | 94.2% |
As can be seen from the table above, the decoking agent has relatively higher decoking rate and better application prospect.
The above description is only exemplary of the present invention and should not be taken as limiting the scope of the present invention, as any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The decoking agent for the boiler is characterized by comprising the following components in parts by mass: 50-80% of nitrate mixture, 10-40% of polymer microspheres and 1-10% of dispersing agent.
2. The boiler decoking agent according to claim 1, wherein the nitrate mixture is a mixture comprising magnesium nitrate, copper nitrate and nickel nitrate.
3. The boiler decoking agent of claim 1, wherein the dispersant is an amphiphilic block copolymer.
5. The boiler decoking agent according to claim 4, wherein the dispersant is prepared by a method comprising the following steps:
(1) respectively carrying out vacuum dehydration on the unit alcohol, the hydroxyl silicone oil and the polyethylene glycol at the temperature of 100-130 ℃, and controlling the moisture content to be less than 0.05 percent;
(2) adding the raw materials and toluene diisocyanate into a reactor, and reacting at 50-80 ℃ until the NCO value is less than 0.03%;
(3) adding succinic anhydride into a reactor, and reacting at 50-80 ℃ until the acid value is less than 10 mgKOH/g;
(4) adding linear polyethyleneimine into a reactor, reacting at the temperature of 100-150 ℃, and simultaneously vacuumizing to remove generated water until the acid value is less than 3 mgKOH/g;
(5) and discharging, cooling and grinding at low temperature into particles to obtain the dispersing agent.
6. The decoking agent for the boiler as claimed in claim 5, wherein the molar ratio of the monoalcohol, the hydroxy silicone oil, the polyethylene glycol, the toluene diisocyanate, the succinic anhydride and the linear polyethyleneimine is 0.2-0.5:1:1-1.2:1.5-2.5:1-1.2: 0.0001-0.0005.
7. The decoking agent for a boiler as claimed in claim 1, wherein the polymer microspheres have an irregular spherical structure consisting of an outer layer and a core layer.
8. The boiler decoking agent of claim 7, wherein the preparation method of the polymer microspheres comprises the following steps:
(1) adding polymerizable monomer containing carbon-carbon double bond, hexadecyl alkane, emulsifier and water into a container, and emulsifying at the rotating speed of 5000-10000 r/min;
(2) respectively putting a photoinitiator and the emulsified liquid prepared in the step (1) into a reactor, and carrying out polymerization reaction at 60-80 ℃;
(3) and after the polymerization is finished, performing centrifugal filtration to obtain the polymer microspheres.
9. The boiler decoking agent of claim 8, wherein the mass ratio of the polymerizable monomer containing carbon-carbon double bond, the hexadecane and the emulsifier is 20-60:40-80:1-5, and the polymerizable monomer containing carbon-carbon double bond is selected from one or more of styrene, methyl styrene, acrylic acid, methacrylic acid, acrylonitrile, glycidyl methacrylate, methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl methacrylate, butyl acrylate, butyl methacrylate, isobornyl methacrylate, vinyl pyrrolidone, vinyl caprolactam, allyl methacrylate and phenyl methacrylate.
10. The decoking agent for the boiler as recited in claim 1, wherein the particle size of the decoking agent for the boiler is 100-300 mesh.
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---|---|---|---|---|
CN115651731A (en) * | 2022-11-10 | 2023-01-31 | 河北德福佳昌化工有限公司 | Ash and coke removing and deslagging agent for boiler |
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