CN103113944B - Method for preparing water-coke slurry - Google Patents
Method for preparing water-coke slurry Download PDFInfo
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- CN103113944B CN103113944B CN201310059669.3A CN201310059669A CN103113944B CN 103113944 B CN103113944 B CN 103113944B CN 201310059669 A CN201310059669 A CN 201310059669A CN 103113944 B CN103113944 B CN 103113944B
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Abstract
The invention provides a method for preparing a water-coke slurry. The method comprises the following steps of: (1) grinding coal, adding the ground coal into the alkaline extract of sodium pyrophosphate, heating, extracting and filtering to obtain a filtrate and a solid retentate; (2) separating precipitates from the filtrate by using an acid, filtering and drying to obtain humic acid; (3) carrying out pyrolysis on the solid retentate to obtain semicoke and coal tar; (4) distilling the coal tar to obtain a coal tar fraction; and (5) mixing and stirring organic bentonite, humic acid, dimethyl silicone oil, the coal tar fraction and deionized water to obtain a slurry, mixing and ball-milling the slurry and the semicoke to obtain the water-coke slurry. The semicoke which is a main product of pyrolysis of the coal is used as a main component, thus the petroleum coke is not used. The method has the outstanding advantages of low cost and wide source of raw materials. The semicoke can be used more widely. The water-coke slurry prepared by adopting the method has excellent flowability and stability and has wide popularization value, and the clean utilization of the semicoke is realized.
Description
Technical field
The invention belongs to clean coal technology field, be specifically related to the preparation method of the burnt slurry of a kind of water.
Background technology
The burnt slurry of water is similar to the effect of coal water slurry, is a kind of particle suspension.Belong to lyophobic dust for raw material-blue charcoal of making the burnt slurry of water, therefore the burnt slurry of water slurry should have good rheological and stability.In order to make the burnt slurry of water during normal use there is lower viscosity and good mobility; When static, have again higher viscosity, be difficult for producing precipitation, in pulping process, generally can add a small amount of chemical additive, consumption is no more than 1% of blue charcoal total amount conventionally.
Application number is that 201120413930.1 Chinese utility model patent discloses a kind of system of utilizing sewage from oil refinery to prepare the burnt slurry of water, the raw material that this patent adopts is the byproduct rock oil coke of refining of petroleum enterprise, in the situation that petroleum resources are in short supply, higher and the difficult acquisition as the price of petroleum coke of by product, and the emphasis of this patent is effective utilization of carrying out sewage from oil refinery.
Application number is that the Chinese invention patent of 200810017478.X discloses water coke slurry for gasification and preparation method thereof, and this patent is also that to adopt refinery coke be raw material, the higher and difficult acquisition of cost of material.
Application number is that 200810012425.9 Chinese invention patent discloses a kind of method of preparing the burnt slurry of water taking lignite semi-coke as raw material, it is raw material that this patent is used the brown coal semicoke that pyrolysis obtains under middle cold condition, the paste consistency of the burnt slurry of made water is 60%, reach the requirement as gasified raw material, but the paste consistency of this patent is consistent with the existing lower-grade metamorphic bituminous concentration of doing coal water slurry, so the standby burnt slurry of water of this patent system does not embody advantage on paste consistency, and consider raw material sources and cost of manufacture, under same condition, lower-grade metamorphic bituminous source is easier, be made into the burnt slurry of water energy consumption lower, chemical reactivity is higher.
In sum, although indivedual patent discloses preparation technology and the method for the burnt slurry of water, in the preparation method of the burnt slurry of existing water, still there is the defects such as raw material sources are limited, tooling cost is high, product chemically reactive is low, seriously hindered development and the application of the burnt slurry of water.
Up to now, not yet finding to adopt the blue charcoal of pyrolysis product of coal is that the correlative study that main raw material is prepared the burnt slurry of water is seen in report.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, and the preparation method of the burnt slurry of a kind of water is provided.It is main ingredient that the method adopts the blue charcoal of the pyrolysis principal product of coal, avoids using refinery coke, has with low cost, raw material sources remarkable advantage widely, makes the application of blue charcoal more extensive; The burnt slurry of water that adopts the method to prepare has good mobility and stability, has reached and has cleaned the object of utilizing blue charcoal, has promotional value widely.
For solving the problems of the technologies described above, the technical solution used in the present invention is: the preparation method of the burnt slurry of a kind of water, it is characterized in that, and the method comprises the following steps:
Step 1, add in trisodium phosphate alkali extract after will coal grinding, in every liter of trisodium phosphate alkali extract, add the coal after 1g～4g grinds, mix to be placed in boiling water bath and heat extracting 2h～2.5h, then carry out filtration treatment, obtain filtrate and solid trapped substance; Described trisodium phosphate alkali extract is mixed by trisodium phosphate, sodium hydroxide and deionized water, and in described trisodium phosphate alkali extract, the concentration of trisodium phosphate is 10g/L～20g/L, and the concentration of sodium hydroxide is 5g/L～10g/L;
Step 2, hydrochloric acid is dropped to and described in step 1, in filtrate, carries out acid out processing, until hold back precipitation without crossing leaching after Precipitation, then by holding back precipitation, to be placed in temperature be that the baking oven of 50 DEG C～70 DEG C is dried, and obtains humic acid;
Step 3, the trapped substance of solid described in step 1 is carried out to pyrolysis processing, the equipment that described pyrolysis processing adopts comprises the nitrogen pot, gas buffer tank, gas meter, pyrolysis oven and the water cooler that connect successively, and the process of described pyrolysis processing is:
Step 301, solid trapped substance is placed in to pyrolysis oven;
Step 302, open nitrogen pot pass into nitrogen in pyrolysis oven, and utilize gas meter to regulate nitrogen flow, making the gaseous tension in pyrolysis oven is 0.3MPa～0.5MPa;
Step 303, be incubated 15min～25min after the solid trapped substance that is placed in pyrolysis oven is warming up to 650 DEG C～800 DEG C carry out pyrolysis processing in step 301, after naturally cooling, in pyrolysis oven, obtain blue charcoal, in water cooler, obtain coal tar;
Step 4, be under the condition of 260 DEG C～300 DEG C, to add thermal distillation to get distillate in temperature by coal tar described in step 303, obtain coal tar fraction;
Step 5, humic acid described in organobentonite and step 2 is added in deionized water, after stirring, add coal tar fraction described in dimethyl silicone oil and step 4, then dispersed with stirring 10min～20min under the condition that is 1500r/min～2500r/min in stir speed (S.S.), obtain slurries, afterwards blue charcoal described in slurries and step 303 is placed in to ball mill ball milling, obtains the burnt slurry of water; In the burnt slurry of described water, the quality percentage composition of blue charcoal is 68%～75%, bentonite quality percentage composition is 0.08%～0.18%, the quality percentage composition of humic acid is 0.14%～1.2%, the quality percentage composition of coal tar fraction is 0.065%～0.75%, the quality percentage composition of dimethyl silicone oil is 0.03%～0.2%, and surplus is deionized water.
The preparation method of the above-mentioned burnt slurry of a kind of water, is characterized in that, coal described in step 1 is bituminous coal.
The preparation method of the above-mentioned burnt slurry of a kind of water, is characterized in that, the size-grade distribution D of coal after grinding in step 1
90be not more than 10 μ m.
The preparation method of the above-mentioned burnt slurry of a kind of water, is characterized in that, the concentration of hydrochloric acid described in step 2 is 0.5mol/L～3mol/L.
The preparation method of the burnt slurry of above-mentioned a kind of water, is characterized in that, the speed heating up described in step 303 is 5 DEG C/min～15 DEG C/min.
The preparation method of the above-mentioned burnt slurry of a kind of water, is characterized in that, the mean particle size of bentonite described in step 5 is not more than 75 μ m.
The preparation method of the above-mentioned burnt slurry of a kind of water, is characterized in that, the speed of ball milling described in step 5 is 300r/min～400r/min, and the time of described ball milling is 10min～20min.
The present invention compared with prior art has the following advantages:
(1) to adopt coal be that raw material is prepared the burnt slurry of water in the present invention, first adopts the method for carry-acid out of alkali that the humic acid in coal is extracted as additive one; Coal after again alkali is carried-acid out is that solid trapped substance carries out pyrolysis processing, during this time by control and optimization to pyrolysis plant and pyrolytic process, obtains the blue charcoal of pyrolysis principal product and pyrolysis byproducts coal tar; Then be to carry out low-temperature distillation under the condition of 260 DEG C～300 DEG C in temperature by coal tar, thereby be partitioned into coal tar fraction as additive two; Adopt afterwards organobentonite as additive three, adopt dimethyl silicone oil as additive four, the mixing and ball milling by the blue charcoal of each additive, pyrolysis principal product with deionized water, finally prepares that paste consistency is high, good fluidity and strong burnt slurry of water of stability.
(2) in the burnt slurry of water that prepared by the present invention, the blue charcoal of main ingredient, additive one humic acid and additive two coal tar fractions are all to make from coal, coal feedstock convenient sources and extensively, and significantly improve the utilization ratio of coal, greatly reduce the traditional problem of environmental pollution that utilizes mode to cause of coal, really accomplished coal to make full use of.
(3) to adopt blue charcoal be the main ingredient of the burnt slurry of water in the present invention, avoids using refinery coke, has low production cost, raw material sources remarkable advantage widely, makes the application of blue charcoal more extensive.
(4) paste consistency of the burnt slurry of water that prepared by the present invention can be up to 68%～75%, paste consistency than the burnt slurry of the water that adopts traditional technology to prepare or coal water slurry has improved 13%～25%, be conducive to the raising of the rear available gas concentration of the burnt slurry gasification of water of the present invention, reach and cleaned the object of utilizing blue charcoal, there is promotional value widely.
(5) viscosity of the burnt slurry of water that prepared by the present invention under 23 DEG C of room temperature conditions is 900mPas～1200mPas, and the burnt slurry of this water is placed and separated out without hard-caked sediment for 25～50 days under 23 DEG C of room temperature conditions, illustrate that the burnt slurry of water prepared by the present invention has good mobility and stability.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Brief description of the drawings
Fig. 1 is preparation technology's schema of the present invention.
Fig. 2 carries out the one-piece construction schematic diagram of equipment that pyrolysis processing adopts for solid trapped substance of the present invention.
Description of reference numerals:
1-nitrogen pot; 2-gas buffer tank; 3-gas meter;
4-pyrolysis oven; 5-water cooler.
Embodiment
As shown in Figure 2, solid trapped substance of the present invention carries out the equipment that pyrolysis processing adopts and comprises the nitrogen pot 1, gas buffer tank 2, gas meter 3, pyrolysis oven 4 and the water cooler 5 that connect successively.
Embodiment 1
In conjunction with Fig. 1 and Fig. 2, the preparation method of the burnt slurry of the present embodiment water comprises the following steps:
Step 1, bituminous coal is carried out to milled processed, make to grind the size-grade distribution D of rear bituminous coal
90be not more than 10 μ m, then the bituminous coal after grinding is added in trisodium phosphate alkali extract, in every liter of trisodium phosphate alkali extract, add the bituminous coal after 2g grinds, mix to be placed on and in boiling water bath, heat extracting 2.5h, finally carry out filtration treatment, obtain filtrate and solid trapped substance; Described trisodium phosphate alkali extract is mixed by trisodium phosphate, sodium hydroxide and deionized water, and in described trisodium phosphate alkali extract, the concentration of trisodium phosphate is 15g/L, and the concentration of sodium hydroxide is 7g/L; The coal analysis data of described bituminous coal are in table 1;
Step 2, the hydrochloric acid that is 1mol/L by concentration drop to and described in step 1, in filtrate, carry out acid out processing, until hold back precipitation without crossing leaching after Precipitation, then by holding back precipitation, to be placed in temperature be that the baking oven of 60 DEG C is dried, and obtains humic acid;
Step 3, the trapped substance of solid described in step 1 is carried out to pyrolysis processing, detailed process is:
Step 301, solid trapped substance is placed in to pyrolysis oven 4;
Step 302, open nitrogen pot 1 pass into nitrogen in pyrolysis oven 4, and utilize gas meter 3 to regulate nitrogen flow, making the gaseous tension in pyrolysis oven 4 is 0.4MPa;
Step 303, be incubated 20min after the solid trapped substance that is placed in pyrolysis oven 4 is heated to 700 DEG C with the temperature rise rate of 10 DEG C/min carry out pyrolysis processing in step 301, after naturally cooling, in pyrolysis oven 4, obtain blue charcoal, in water cooler 5, obtain coal tar;
Step 4, be under the condition of 280 DEG C, to add thermal distillation to get distillate in temperature by coal tar described in step 303, obtain coal tar fraction;
Step 5, mean particle size is not more than to humic acid described in the organobentonite of 75 μ m and step 2 adds in deionized water, after stirring, add coal tar fraction described in dimethyl silicone oil and step 4, then dispersed with stirring 15min under the condition that is 2000r/min in stir speed (S.S.), obtain slurries, afterwards blue charcoal described in slurries and step 303 is placed in to planetary ball mill, with the speed ball milling 15min of 350r/min, obtain the burnt slurry of water; In the burnt slurry of described water, the quality percentage composition of blue charcoal is 68%, bentonite quality percentage composition is 0.08%, the quality percentage composition of humic acid is 0.28%, the quality percentage composition of coal tar fraction is 0.068%, the quality percentage composition of dimethyl silicone oil is 0.04%, and surplus is deionized water.
The coal analysis data of table 1 the present embodiment bituminous coal
In table, each letter represents respectively: C
daf: carbon content in coal content (dry ash-free basis); H
daf: hydrogen content in coal (dry ash-free basis); N
daf: nitrogen content of coal content (dry ash-free basis); O
daf: oxygen content of coal content (dry ash-free basis); S
daf: sulfur content of coal (dry ash-free basis); M
ad: moisture in coal content (air dried basis); A
ad: ash oontent in coal (air dried basis); V
daf: volatile content in coal (dry ash-free basis); FC
ad: fixed carbon content (air dried basis) in coal; Lower same.
The test data of the pyrogenous origin blue charcoal of the present embodiment is: fixed carbon content 81.59wt%, volatile matter 9.67wt%, ash content 7.04wt%, total water 16.04wt%, sulphur content 0.3wt%.
The viscosity of the burnt slurry of water prepared by the present embodiment under 23 DEG C of room temperature conditions is 950mPas, and the burnt slurry of this water places and separate out without hard-caked sediment for 40 days under 23 DEG C of room temperature conditions, illustrate that burnt slurry of water prepared by the present embodiment has good mobility and stability.
Embodiment 2
In conjunction with Fig. 1 and Fig. 2, the preparation method of the burnt slurry of the present embodiment water comprises the following steps:
Step 1, bituminous coal is carried out to milled processed, make to grind the size-grade distribution D of rear bituminous coal
90be not more than 10 μ m, then the bituminous coal after grinding is added in trisodium phosphate alkali extract, in every liter of trisodium phosphate alkali extract, add the bituminous coal after 3g grinds, mix to be placed on and in boiling water bath, heat extracting 2h, finally carry out filtration treatment, obtain filtrate and solid trapped substance; Described trisodium phosphate alkali extract is mixed by trisodium phosphate, sodium hydroxide and deionized water, and in described trisodium phosphate alkali extract, the concentration of trisodium phosphate is 16g/L, and the concentration of sodium hydroxide is 8g/L; The coal analysis data of described bituminous coal are in table 2;
Step 2, the hydrochloric acid that is 0.8mol/L by concentration drop to and described in step 1, in filtrate, carry out acid out processing, until hold back precipitation without crossing leaching after Precipitation, then by holding back precipitation, to be placed in temperature be that the baking oven of 65 DEG C is dried, and obtains humic acid;
Step 3, the trapped substance of solid described in step 1 is carried out to pyrolysis processing, detailed process is:
Step 301, solid trapped substance is placed in to pyrolysis oven 4;
Step 302, open nitrogen pot 1 pass into nitrogen in pyrolysis oven 4, and utilize gas meter 3 to regulate nitrogen flow, making the gaseous tension in pyrolysis oven 4 is 0.4MPa;
Step 303, be incubated 18min after the solid trapped substance that is placed in pyrolysis oven 4 is heated to 720 DEG C with the temperature rise rate of 8 DEG C/min carry out pyrolysis processing in step 301, after naturally cooling, in pyrolysis oven 4, obtain blue charcoal, in water cooler 5, obtain coal tar;
Step 4, be under the condition of 270 DEG C, to add thermal distillation to get distillate in temperature by coal tar described in step 303, obtain coal tar fraction;
Step 5, mean particle size is not more than to humic acid described in the organobentonite of 75 μ m and step 2 adds in deionized water, after stirring, add coal tar fraction described in dimethyl silicone oil and step 4, then dispersed with stirring 10min under the condition that is 2200r/min in stir speed (S.S.), obtain slurries, afterwards blue charcoal described in slurries and step 303 is placed in to planetary ball mill, with the speed ball milling 18min of 320r/min, obtain the burnt slurry of water; In the burnt slurry of described water, the quality percentage composition of blue charcoal is 72%, bentonite quality percentage composition is 0.09%, the quality percentage composition of humic acid is 0.65%, the quality percentage composition of coal tar fraction is 0.11%, the quality percentage composition of dimethyl silicone oil is 0.08%, and surplus is deionized water.
The coal analysis data of table 2 the present embodiment bituminous coal
The test data of the pyrogenous origin blue charcoal of the present embodiment is: fixed carbon content 81.73wt%, volatile matter 9.91wt%, ash content 8.88wt%, total water 17.71wt%, sulphur content 0.32wt%.
The viscosity of the burnt slurry of water prepared by the present embodiment under 23 DEG C of room temperature conditions is 1100mPas, and the burnt slurry of this water places and separate out without hard-caked sediment for 30 days under 23 DEG C of room temperature conditions, illustrate that burnt slurry of water prepared by the present embodiment has good mobility and stability.
Embodiment 3
In conjunction with Fig. 1 and Fig. 2, the preparation method of the burnt slurry of the present embodiment water comprises the following steps:
Step 1, bituminous coal is carried out to milled processed, make to grind the size-grade distribution D of rear bituminous coal
90be not more than 10 μ m, then the bituminous coal after grinding is added in trisodium phosphate alkali extract, in every liter of trisodium phosphate alkali extract, add the bituminous coal after 1g grinds, mix to be placed on and in boiling water bath, heat extracting 2h, finally carry out filtration treatment, obtain filtrate and solid trapped substance; Described trisodium phosphate alkali extract is mixed by trisodium phosphate, sodium hydroxide and deionized water, and in described trisodium phosphate alkali extract, the concentration of trisodium phosphate is 20g/L, and the concentration of sodium hydroxide is 10g/L; The coal analysis data of described bituminous coal are in table 3;
Step 2, the hydrochloric acid that is 2mol/L by concentration drop to and described in step 1, in filtrate, carry out acid out processing, until hold back precipitation without crossing leaching after Precipitation, then by holding back precipitation, to be placed in temperature be that the baking oven of 55 DEG C is dried, and obtains humic acid;
Step 3, the trapped substance of solid described in step 1 is carried out to pyrolysis processing, detailed process is:
Step 301, solid trapped substance is placed in to pyrolysis oven 4;
Step 302, open nitrogen pot 1 pass into nitrogen in pyrolysis oven 4, and utilize gas meter 3 to regulate nitrogen flow, making the gaseous tension in pyrolysis oven 4 is 0.5MPa;
Step 303, be incubated 20min after the solid trapped substance that is placed in pyrolysis oven 4 is heated to 750 DEG C with the temperature rise rate of 12 DEG C/min carry out pyrolysis processing in step 301, after naturally cooling, in pyrolysis oven 4, obtain blue charcoal, in water cooler 5, obtain coal tar;
Step 4, be under the condition of 300 DEG C, to add thermal distillation to get distillate in temperature by coal tar described in step 303, obtain coal tar fraction;
Step 5, mean particle size is not more than to humic acid described in the organobentonite of 75 μ m and step 2 adds in deionized water, after stirring, add coal tar fraction described in dimethyl silicone oil and step 4, then dispersed with stirring 15min under the condition that is 2500r/min in stir speed (S.S.), obtain slurries, afterwards blue charcoal described in slurries and step 303 is placed in to planetary ball mill, with the speed ball milling 12min of 380r/min, obtain the burnt slurry of water; In the burnt slurry of described water, the quality percentage composition of blue charcoal is 75%, bentonite quality percentage composition is 0.13%, the quality percentage composition of humic acid is 0.96%, the quality percentage composition of coal tar fraction is 0.17%, the quality percentage composition of dimethyl silicone oil is 0.12%, and surplus is deionized water.
The coal analysis data of table 3 the present embodiment bituminous coal
The test data of the pyrogenous origin blue charcoal of the present embodiment is: fixed carbon content 82.31wt%, volatile matter 10.15wt%, ash content 7.94wt%, total water 18.40wt%, sulphur content 0.45wt%.
The viscosity of the burnt slurry of water prepared by the present embodiment under 23 DEG C of room temperature conditions is 1150mPas, and the burnt slurry of this water places and separate out without hard-caked sediment for 38 days under 23 DEG C of room temperature conditions, illustrate that burnt slurry of water prepared by the present embodiment has good mobility and stability.
Embodiment 4
In conjunction with Fig. 1 and Fig. 2, the preparation method of the burnt slurry of the present embodiment water comprises the following steps:
Step 1, bituminous coal is carried out to milled processed, make to grind the size-grade distribution D of rear bituminous coal
90be not more than 10 μ m, then the bituminous coal after grinding is added in trisodium phosphate alkali extract, in every liter of trisodium phosphate alkali extract, add the bituminous coal after 4g grinds, mix to be placed on and in boiling water bath, heat extracting 2h, finally carry out filtration treatment, obtain filtrate and solid trapped substance; Described trisodium phosphate alkali extract is mixed by trisodium phosphate, sodium hydroxide and deionized water, and in described trisodium phosphate alkali extract, the concentration of trisodium phosphate is 12g/L, and the concentration of sodium hydroxide is 9g/L; The coal analysis data of described bituminous coal are in table 4;
Step 2, the hydrochloric acid that is 2.1mol/L by concentration drop to and described in step 1, in filtrate, carry out acid out processing, until hold back precipitation without crossing leaching after Precipitation, then by holding back precipitation, to be placed in temperature be that the baking oven of 70 DEG C is dried, and obtains humic acid;
Step 3, the trapped substance of solid described in step 1 is carried out to pyrolysis processing, detailed process is:
Step 301, solid trapped substance is placed in to pyrolysis oven 4;
Step 302, open nitrogen pot 1 pass into nitrogen in pyrolysis oven 4, and utilize gas meter 3 to regulate nitrogen flow, making the gaseous tension in pyrolysis oven 4 is 0.3MPa;
Step 303, be incubated 25min after the solid trapped substance that is placed in pyrolysis oven 4 is heated to 780 DEG C with the temperature rise rate of 6 DEG C/min carry out pyrolysis processing in step 301, after naturally cooling, in pyrolysis oven 4, obtain blue charcoal, in water cooler 5, obtain coal tar;
Step 4, be under the condition of 260 DEG C, to add thermal distillation to get distillate in temperature by coal tar described in step 303, obtain coal tar fraction;
Step 5, mean particle size is not more than to humic acid described in the organobentonite of 75 μ m and step 2 adds in deionized water, after stirring, add coal tar fraction described in dimethyl silicone oil and step 4, then dispersed with stirring 10min under the condition that is 2500r/min in stir speed (S.S.), obtain slurries, afterwards blue charcoal described in slurries and step 303 is placed in to planetary ball mill, with the speed ball milling 10min of 400r/min, obtain the burnt slurry of water; In the burnt slurry of described water, the quality percentage composition of blue charcoal is 69%, bentonite quality percentage composition is 0.16%, and the quality percentage composition of humic acid is 0.8%, and the quality percentage composition of coal tar fraction is 0.6%, the quality percentage composition of dimethyl silicone oil is 0.1%, and surplus is deionized water.
The coal analysis data of table 4 the present embodiment bituminous coal
The test data of the pyrogenous origin blue charcoal of the present embodiment is: fixed carbon content 81.89wt%, volatile matter 10.37wt%, ash content 7.68wt%, total water 19.15wt%, sulphur content 0.27wt%.
The viscosity of the burnt slurry of water prepared by the present embodiment under 23 DEG C of room temperature conditions is 900mPas, and the burnt slurry of this water places and separate out without hard-caked sediment for 50 days under 23 DEG C of room temperature conditions, illustrate that burnt slurry of water prepared by the present embodiment has good mobility and stability.
Embodiment 5
In conjunction with Fig. 1 and Fig. 2, the preparation method of the burnt slurry of the present embodiment water comprises the following steps:
Step 1, bituminous coal is carried out to milled processed, make to grind the size-grade distribution D of rear bituminous coal
90be not more than 10 μ m, then the bituminous coal after grinding is added in trisodium phosphate alkali extract, in every liter of trisodium phosphate alkali extract, add the bituminous coal after 4g grinds, mix to be placed on and in boiling water bath, heat extracting 2h, finally carry out filtration treatment, obtain filtrate and solid trapped substance; Described trisodium phosphate alkali extract is mixed by trisodium phosphate, sodium hydroxide and deionized water, and in described trisodium phosphate alkali extract, the concentration of trisodium phosphate is 20g/L, and the concentration of sodium hydroxide is 5g/L; The coal analysis data of described bituminous coal are in table 5;
Step 2, the hydrochloric acid that is 0.5mol/L by concentration drop to and described in step 1, in filtrate, carry out acid out processing, until hold back precipitation without crossing leaching after Precipitation, then by holding back precipitation, to be placed in temperature be that the baking oven of 50 DEG C is dried, and obtains humic acid;
Step 3, the trapped substance of solid described in step 1 is carried out to pyrolysis processing, detailed process is:
Step 301, solid trapped substance is placed in to pyrolysis oven 4;
Step 302, open nitrogen pot 1 pass into nitrogen in pyrolysis oven 4, and utilize gas meter 3 to regulate nitrogen flow, making the gaseous tension in pyrolysis oven 4 is 0.5MPa;
Step 303, be incubated 25min after the solid trapped substance that is placed in pyrolysis oven 4 is heated to 800 DEG C with the temperature rise rate of 15 DEG C/min carry out pyrolysis processing in step 301, after naturally cooling, in pyrolysis oven 4, obtain blue charcoal, in water cooler 5, obtain coal tar;
Step 4, be under the condition of 260 DEG C, to add thermal distillation to get distillate in temperature by coal tar described in step 303, obtain coal tar fraction;
Step 5, mean particle size is not more than to humic acid described in the organobentonite of 75 μ m and step 2 adds in deionized water, after stirring, add coal tar fraction described in dimethyl silicone oil and step 4, then dispersed with stirring 20min under the condition that is 1500r/min in stir speed (S.S.), obtain slurries, afterwards blue charcoal described in slurries and step 303 is placed in to planetary ball mill, with the speed ball milling 20min of 400r/min, obtain the burnt slurry of water; In the burnt slurry of described water, the quality percentage composition of blue charcoal is 72%, bentonite quality percentage composition is 0.12%, and the quality percentage composition of humic acid is 1.0%, and the quality percentage composition of coal tar fraction is 0.6%, the quality percentage composition of dimethyl silicone oil is 0.1%, and surplus is deionized water.
The coal analysis data of table 5 the present embodiment bituminous coal
The test data of the pyrogenous origin blue charcoal of the present embodiment is: fixed carbon content 83.21wt%, volatile matter 9.99wt%, ash content 7.85wt%, total water 18.59wt%, sulphur content 0.15wt%.
The viscosity of the burnt slurry of water prepared by the present embodiment under 23 DEG C of room temperature conditions is 980mPas, and the burnt slurry of this water places and separate out without hard-caked sediment for 34 days under 23 DEG C of room temperature conditions, illustrate that burnt slurry of water prepared by the present embodiment has good mobility and stability.
Embodiment 6
In conjunction with Fig. 1 and Fig. 2, the preparation method of the burnt slurry of the present embodiment water comprises the following steps:
Step 1, bituminous coal is carried out to milled processed, make to grind the size-grade distribution D of rear bituminous coal
90be not more than 10 μ m, then the bituminous coal after grinding is added in trisodium phosphate alkali extract, in every liter of trisodium phosphate alkali extract, add the bituminous coal after 4g grinds, mix to be placed on and in boiling water bath, heat extracting 2h, finally carry out filtration treatment, obtain filtrate and solid trapped substance; Described trisodium phosphate alkali extract is mixed by trisodium phosphate, sodium hydroxide and deionized water, and in described trisodium phosphate alkali extract, the concentration of trisodium phosphate is 20g/L, and the concentration of sodium hydroxide is 10g/L; The coal analysis data of described bituminous coal are in table 6;
Step 2, the hydrochloric acid that is 3mol/L by concentration drop to and described in step 1, in filtrate, carry out acid out processing, until hold back precipitation without crossing leaching after Precipitation, then by holding back precipitation, to be placed in temperature be that the baking oven of 58 DEG C is dried, and obtains humic acid;
Step 3, the trapped substance of solid described in step 1 is carried out to pyrolysis processing, detailed process is:
Step 301, solid trapped substance is placed in to pyrolysis oven 4;
Step 302, open nitrogen pot 1 pass into nitrogen in pyrolysis oven 4, and utilize gas meter 3 to regulate nitrogen flow, making the gaseous tension in pyrolysis oven 4 is 0.5MPa;
Step 303, be incubated 25min after the solid trapped substance that is placed in pyrolysis oven 4 is heated to 650 DEG C with the temperature rise rate of 15 DEG C/min carry out pyrolysis processing in step 301, after naturally cooling, in pyrolysis oven 4, obtain blue charcoal, in water cooler 5, obtain coal tar;
Step 4, be under the condition of 300 DEG C, to add thermal distillation to get distillate in temperature by coal tar described in step 303, obtain coal tar fraction;
Step 5, mean particle size is not more than to humic acid described in the organobentonite of 75 μ m and step 2 adds in deionized water, after stirring, add coal tar fraction described in dimethyl silicone oil and step 4, then dispersed with stirring 10min under the condition that is 2500r/min in stir speed (S.S.), obtain slurries, afterwards blue charcoal described in slurries and step 303 is placed in to planetary ball mill, with the speed ball milling 20min of 300r/min, obtain the burnt slurry of water; In the burnt slurry of described water, the quality percentage composition of blue charcoal is 70%, bentonite quality percentage composition is 0.08%, and the quality percentage composition of humic acid is 1.2%, and the quality percentage composition of coal tar fraction is 0.75%, the quality percentage composition of dimethyl silicone oil is 0.2%, and surplus is deionized water.
The coal analysis data of table 6 the present embodiment bituminous coal
The test data of the pyrogenous origin blue charcoal of the present embodiment is: fixed carbon content 80.99wt%, volatile matter 10.31wt%, ash content 7.68wt%, total water 18.32wt%, sulphur content 0.41wt%.
The viscosity of the burnt slurry of water prepared by the present embodiment under 23 DEG C of room temperature conditions is 1000mPas, and the burnt slurry of this water places and separate out without hard-caked sediment for 35 days under 23 DEG C of room temperature conditions, illustrate that burnt slurry of water prepared by the present embodiment has good mobility and stability.
Embodiment 7
In conjunction with Fig. 1 and Fig. 2, the preparation method of the burnt slurry of the present embodiment water comprises the following steps:
Step 1, bituminous coal is carried out to milled processed, make to grind the size-grade distribution D of rear bituminous coal
90be not more than 10 μ m, then the bituminous coal after grinding is added in trisodium phosphate alkali extract, in every liter of trisodium phosphate alkali extract, add the bituminous coal after 1g grinds, mix to be placed on and in boiling water bath, heat extracting 2.5h, finally carry out filtration treatment, obtain filtrate and solid trapped substance; Described trisodium phosphate alkali extract is mixed by trisodium phosphate, sodium hydroxide and deionized water, and in described trisodium phosphate alkali extract, the concentration of trisodium phosphate is 10g/L, and the concentration of sodium hydroxide is 5g/L; The coal analysis data of described bituminous coal are in table 7;
Step 2, the hydrochloric acid that is 0.5mol/L by concentration drop to and described in step 1, in filtrate, carry out acid out processing, until hold back precipitation without crossing leaching after Precipitation, then by holding back precipitation, to be placed in temperature be that the baking oven of 50 DEG C is dried, and obtains humic acid;
Step 3, the trapped substance of solid described in step 1 is carried out to pyrolysis processing, detailed process is:
Step 301, solid trapped substance is placed in to pyrolysis oven 4;
Step 302, open nitrogen pot 1 pass into nitrogen in pyrolysis oven 4, and utilize gas meter 3 to regulate nitrogen flow, making the gaseous tension in pyrolysis oven 4 is 0.3MPa;
Step 303, be incubated 15min after the solid trapped substance that is placed in pyrolysis oven 4 is heated to 800 DEG C with the temperature rise rate of 5 DEG C/min carry out pyrolysis processing in step 301, after naturally cooling, in pyrolysis oven 4, obtain blue charcoal, in water cooler 5, obtain coal tar;
Step 4, be under the condition of 260 DEG C, to add thermal distillation to get distillate in temperature by coal tar described in step 303, obtain coal tar fraction;
Step 5, mean particle size is not more than to humic acid described in the organobentonite of 75 μ m and step 2 adds in deionized water, after stirring, add coal tar fraction described in dimethyl silicone oil and step 4, then dispersed with stirring 20min under the condition that is 1500r/min in stir speed (S.S.), obtain slurries, afterwards blue charcoal described in slurries and step 303 is placed in to planetary ball mill, with the speed ball milling 10min of 400r/min, obtain the burnt slurry of water; In the burnt slurry of described water, the quality percentage composition of blue charcoal is 75%, bentonite quality percentage composition is 0.18%, the quality percentage composition of humic acid is 0.14%, the quality percentage composition of coal tar fraction is 0.065%, the quality percentage composition of dimethyl silicone oil is 0.03%, and surplus is deionized water.
The coal analysis data of table 7 the present embodiment bituminous coal
The test data of the pyrogenous origin blue charcoal of the present embodiment is: fixed carbon content 81.98wt%, volatile matter 10.13wt%, ash content 7.59wt%, total water 18.65wt%, sulphur content 0.36wt%.
The viscosity of the burnt slurry of water prepared by the present embodiment under 23 DEG C of room temperature conditions is 1200mPas, and the burnt slurry of this water places and separate out without hard-caked sediment for 25 days under 23 DEG C of room temperature conditions, illustrate that burnt slurry of water prepared by the present embodiment has good mobility and stability.
Embodiment 8
In conjunction with Fig. 1 and Fig. 2, the preparation method of the burnt slurry of the present embodiment water comprises the following steps:
Step 1, bituminous coal is carried out to milled processed, make to grind the size-grade distribution D of rear bituminous coal
90be not more than 10 μ m, then the bituminous coal after grinding is added in trisodium phosphate alkali extract, in every liter of trisodium phosphate alkali extract, add the bituminous coal after 3.5g grinds, mix to be placed on and in boiling water bath, heat extracting 2h, finally carry out filtration treatment, obtain filtrate and solid trapped substance; Described trisodium phosphate alkali extract is mixed by trisodium phosphate, sodium hydroxide and deionized water, and in described trisodium phosphate alkali extract, the concentration of trisodium phosphate is 12g/L, and the concentration of sodium hydroxide is 8g/L; The coal analysis data of described bituminous coal are in table 8;
Step 2, the hydrochloric acid that is 2.5mol/L by concentration drop to and described in step 1, in filtrate, carry out acid out processing, until hold back precipitation without crossing leaching after Precipitation, then by holding back precipitation, to be placed in temperature be that the baking oven of 50 DEG C is dried, and obtains humic acid;
Step 3, the trapped substance of solid described in step 1 is carried out to pyrolysis processing, detailed process is:
Step 301, solid trapped substance is placed in to pyrolysis oven 4;
Step 302, open nitrogen pot 1 pass into nitrogen in pyrolysis oven 4, and utilize gas meter 3 to regulate nitrogen flow, making the gaseous tension in pyrolysis oven 4 is 0.5MPa;
Step 303, be incubated 15min after the solid trapped substance that is placed in pyrolysis oven 4 is heated to 650 DEG C with the temperature rise rate of 5 DEG C/min carry out pyrolysis processing in step 301, after naturally cooling, in pyrolysis oven 4, obtain blue charcoal, in water cooler 5, obtain coal tar;
Step 4, be under the condition of 290 DEG C, to add thermal distillation to get distillate in temperature by coal tar described in step 303, obtain coal tar fraction;
Step 5, mean particle size is not more than to humic acid described in the organobentonite of 75 μ m and step 2 adds in deionized water, after stirring, add coal tar fraction described in dimethyl silicone oil and step 4, then dispersed with stirring 20min under the condition that is 2500r/min in stir speed (S.S.), obtain slurries, afterwards blue charcoal described in slurries and step 303 is placed in to planetary ball mill, with the speed ball milling 20min of 400r/min, obtain the burnt slurry of water; In the burnt slurry of described water, the quality percentage composition of blue charcoal is 74%, bentonite quality percentage composition is 0.15%, the quality percentage composition of humic acid is 0.5%, the quality percentage composition of coal tar fraction is 0.45%, the quality percentage composition of dimethyl silicone oil is 0.09%, and surplus is deionized water.
The coal analysis data of table 8 the present embodiment bituminous coal
The test data of the pyrogenous origin blue charcoal of the present embodiment is: fixed carbon content 80.45wt%, volatile matter 10.35wt%, ash content 7.63wt%, total water 18.44wt%, sulphur content 0.38wt%.
The viscosity of the burnt slurry of water prepared by the present embodiment under 23 DEG C of room temperature conditions is 1180mPas, and the burnt slurry of this water places and separate out without hard-caked sediment for 45 days under 23 DEG C of room temperature conditions, illustrate that burnt slurry of water prepared by the present embodiment has good mobility and stability.
The above, be only preferred embodiment of the present invention, not the present invention imposed any restrictions.Every any simple modification of above embodiment being done according to invention technical spirit, change and equivalence change, and all still belong in the protection domain of technical solution of the present invention.
Claims (7)
1. a preparation method for the burnt slurry of water, is characterized in that, the method comprises the following steps:
Step 1, add in trisodium phosphate alkali extract after will coal grinding, in every liter of trisodium phosphate alkali extract, add the coal after 1g～4g grinds, mix to be placed in boiling water bath and heat extracting 2h～2.5h, then carry out filtration treatment, obtain filtrate and solid trapped substance; Described trisodium phosphate alkali extract is mixed by trisodium phosphate, sodium hydroxide and deionized water, and in described trisodium phosphate alkali extract, the concentration of trisodium phosphate is 10g/L～20g/L, and the concentration of sodium hydroxide is 5g/L～10g/L;
Step 2, hydrochloric acid is dropped to and described in step 1, in filtrate, carries out acid out processing, until hold back precipitation without crossing leaching after Precipitation, then by holding back precipitation, to be placed in temperature be that the baking oven of 50 DEG C～70 DEG C is dried, and obtains humic acid;
Step 3, the trapped substance of solid described in step 1 is carried out to pyrolysis processing, the equipment that described pyrolysis processing adopts comprises the nitrogen pot (1), gas buffer tank (2), gas meter (3), pyrolysis oven (4) and the water cooler (5) that connect successively, and the process of described pyrolysis processing is:
Step 301, solid trapped substance is placed in to pyrolysis oven (4);
Step 302, open nitrogen pot (1) pass into nitrogen in pyrolysis oven (4), and utilize gas meter (3) to regulate nitrogen flow, making the gaseous tension in pyrolysis oven (4) is 0.3MPa～0.5MPa;
Step 303, be incubated 15min～25min after the solid trapped substance that is placed in pyrolysis oven (4) is warming up to 650 DEG C～800 DEG C carry out pyrolysis processing in step 301, after naturally cooling, in pyrolysis oven (4), obtain blue charcoal, in water cooler (5), obtain coal tar;
Step 4, be under the condition of 260 DEG C～300 DEG C, to add thermal distillation to get distillate in temperature by coal tar described in step 303, obtain coal tar fraction;
Step 5, humic acid described in organobentonite and step 2 is added in deionized water, after stirring, add coal tar fraction described in dimethyl silicone oil and step 4, then dispersed with stirring 10min～20min under the condition that is 1500r/min～2500r/min in stir speed (S.S.), obtain slurries, afterwards blue charcoal described in slurries and step 303 is placed in to ball mill ball milling, obtains the burnt slurry of water; In the burnt slurry of described water, the quality percentage composition of blue charcoal is 68%～75%, bentonite quality percentage composition is 0.08%～0.18%, the quality percentage composition of humic acid is 0.14%～1.2%, the quality percentage composition of coal tar fraction is 0.065%～0.75%, the quality percentage composition of dimethyl silicone oil is 0.03%～0.2%, and surplus is deionized water.
2. the preparation method of the burnt slurry of a kind of water according to claim 1, is characterized in that, coal described in step 1 is bituminous coal.
3. the preparation method of the burnt slurry of a kind of water according to claim 1, is characterized in that, the size-grade distribution D of coal after grinding in step 1
90be not more than 10 μ m.
4. the preparation method of the burnt slurry of a kind of water according to claim 1, is characterized in that, the concentration of hydrochloric acid described in step 2 is 0.5mol/L～3mol/L.
5. the preparation method of the burnt slurry of a kind of water according to claim 1, is characterized in that, the speed heating up described in step 303 is 5 DEG C/min～15 DEG C/min.
6. the preparation method of the burnt slurry of a kind of water according to claim 1, is characterized in that, the mean particle size of bentonite described in step 5 is not more than 75 μ m.
7. the preparation method of the burnt slurry of a kind of water according to claim 1, is characterized in that, the speed of ball milling described in step 5 is 300r/min～400r/min, and the time of described ball milling is 10min～20min.
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