CN105268461A - Method for recovering lignin from straw pulp black liquid to prepare lignin carbon carrier catalyst - Google Patents
Method for recovering lignin from straw pulp black liquid to prepare lignin carbon carrier catalyst Download PDFInfo
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- CN105268461A CN105268461A CN201510739463.4A CN201510739463A CN105268461A CN 105268461 A CN105268461 A CN 105268461A CN 201510739463 A CN201510739463 A CN 201510739463A CN 105268461 A CN105268461 A CN 105268461A
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Abstract
The invention discloses a method for recovering lignin from straw pulp black liquid to prepare a lignin carbon carrier catalyst, and belongs to the technical field of catalysts. According to the method, papermaking straw pulp black liquid is used as raw materials and is put into a high-pressure tank; then, boiler flue gas is introduced for acidification; performing aeration to collect lignin crude products; active sludge is used for fermentation; absolute ethyl alcohol is added; a Buchner funnel is used for filter pressing to obtain pure lignin; the lignin is carbonized and is then mixed with potassium carbonate to be ground; the ground materials are put into a tubular reactor for activation; then, the lignin carbon carrier catalyst prepared from the lignin recovered from the straw pulp black liquid is obtained. The method has the advantages that the papermaking straw pulp black liquid is fully and reasonably utilized; prepared lignin particles are uniform; the performance is excellent; in addition, the waste liquid quantity is greatly reduced; the environment pollution is reduced; the activity of the prepared catalyst is improved, so that the reaction time is reduced by 20 to 30 percent.
Description
Technical field
The invention discloses a kind of method reclaiming lignin and prepare lignin high-area carbon catalyst from straw pulp black liquor, belong to catalyst technical field.
Background technology
In modern chemical industry industry, acid catalyst is absolutely necessary, be widely used in the various fields such as pharmacy, petro chemical industry, macromolecule chemical industry, but the catalyst used at present is mostly the liquid acid catalyst such as hydrochloric acid, sulfuric acid and brings product separation difficulty, be difficult to reuse and the problems such as environmental pollution.
Paper-making industry is the heavy polluted industry of China, and wherein most important reason is exactly the process of black liquid.Under normal circumstances, enterprise generally adopts two kinds of methods to black liquor treatment: one carries out concentrated burning to black liquor; Another kind utilizes black liquor to develop lignin product.Front kind of method black liquor is through condensed combustion, although the alkali that can reclaim in black liquor and part calorific value, is a kind of low value Land use systems concerning alkali lignin, and equipment investment large, consume energy high.A kind of rear method is by carrying out chemical modification to alkali lignin, develop lignified chemical product, improving its high added value, is the good method of Appropriate application alkali lignin, is also the fundamental solution utilizing black liquid on a large scale, alleviate also final elimination paper-making black liquor simultaneously.Therefore, lignin production obtains as process black liquor of pulp making and profit new growth point and admits widely and adopt.
Lignin how in Appropriate application black liquor, topmost difficult point is exactly the extraction process of lignin.Containing of black liquor is consolidated in thing, except lignin, also have the impurity such as reduced sugar, Small molecular inorganic salts and cellulose, the existence of these impurity, considerable influence is had to the dispersiveness of dye dispersant and heat endurance, make extraction process very complicated, and serious for environmental pollution in leaching process, the lignin particles extracted is uneven.The raw material restriction used due to domestic dye dispersant and process technology level not high, the high-performance dye dispersant that domestic dyestuff producer uses for this reason is mainly derived from imported product.
Summary of the invention
The technical problem that the present invention mainly solves: for adopting burning method concerning being that low value utilizes lignin in current straw pulp black liquor processing procedure, and equipment investment and power consumption high, and current inorganic acid out precipitation extraction lignin purity is not high, and easily cause secondary pollution, the shortcoming that cost is high, provides a kind of method reclaiming lignin and prepare lignin high-area carbon catalyst from straw pulp black liquor.The method take paper-making black liquid as raw material, put into pressure pan and pass into boiler flue and carry out acidifying, aeration collects the thick product of lignin, ferment with activated sludge, add the press filtration of absolute ethyl alcohol Buchner funnel and obtain pure lignin, carbonized wood quality grind after mixing with potash afterwards, puts into namely to obtain after tubular reactor activates and a kind ofly reclaims lignin high-area carbon catalyst prepared by lignin from straw pulp black liquor.The method has carried out adequately and reasonably utilizing to paper-making black liquid, and the lignin particles not only made is even, excellent performance, and greatly reduces waste liquid amount, decreases environmental pollution.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) get 3 ~ 4L paper-making black liquid and remove the impurity such as fine fibre by strainer filtering, pour in higfh-tension ceramics tank afterwards, the boiler flue through dedusting humidification is passed in tank, until pressure reaches 180 ~ 190kPa in higfh-tension ceramics pressure tank table display tank, after keeping stress reaction 12 ~ 18h, make black liquor acidifying;
(2) open pressure pan pressure-reducing valve, the black liquor after boiler flue gas disposal is moved into bottom with in the aeration tank of aerator, open aeration valve and carry out aeration, at the thick product of aeration tank surface collection lignin;
(3) thick for lignin product is moved into fermentation tank, inoculate the activated sludge obtained from secondary sedimentation tank of sewage treatment work wherein, activated sludge inoculum concentration is 15 ~ 20% of lignin crude product gross mass, add the thiosulfuric acid sodium crystal of lignin total amount 2 ~ 5% afterwards again, incubator is put into, 40 ~ 50 DEG C of bottom fermentations 4 ~ 5 days after being sealed by fermentation tank mouth preservative film;
(4) fermentate is moved into beaker, add the absolute ethyl alcohol of fermentate 3 times of volumes, be placed on magnetic stirrer, stir 10 ~ 20min with the rotating speed of 500 ~ 600r/min and obtain mixed liquor, mixed liquor is moved into cloth filter press, press filtration, obtain filtrate, filtrate is moved into water-bath, is warming up to 80 ~ 90 DEG C, pure lignin is separated out in distillation;
(5) lignin of above-mentioned recovery is put into retort, first be warming up to 70 ~ 80 DEG C with the rate program of 5 DEG C/min, insulation 10 ~ 20min carbonizes in advance, then is warming up to 200 ~ 300 DEG C with the rate program of 8 DEG C/min, insulation charing 40 ~ 60min, obtains carbonized wood quality;
(6) by carbonized wood quality obtained above and potash in mass ratio for 3:4 mix after put into mortar and grind, blend after mixing is put into stainless steel tubular reactor, and tubular reactor is put into horizontal tube resistance furnace, by ramp to 80 ~ 90 DEG C of room temperature by 10 DEG C/min, insulation activation 2 ~ 3h, Temperature fall is to room temperature under nitrogen atmosphere again, and whole process nitrogen intake is 80 ~ 100cm
3, namely obtain a kind of lignin high-area carbon catalyst reclaiming lignin and prepare from straw pulp black liquor.
Application process of the present invention is: be used in the course of reaction of vegetable oil production biodiesel by the catalytic lignin agent obtained by the present invention, wherein, use amount is for adding the catalyst obtained by 5 ~ 8g the present invention in every 3 ~ 5kg reaction bed material oil, finally record, with do not add compared with catalyst that the present invention obtains, the reaction time decreases 20 ~ 30%.
The invention has the beneficial effects as follows:
(1) the present invention has carried out adequately and reasonably utilizing to paper-making black liquid, and the lignin particles made is even, excellent performance;
(2) the present invention not only greatly reduces waste liquid amount, and makes the waste water producing lignin neutral simultaneously, and suspension is low, and waste water reaches standard;
(3) catalyst activity made by improves, excellent catalytic effect, and pore structure is flourishing, good stability.
Detailed description of the invention
First get 3 ~ 4L paper-making black liquid and remove the impurity such as fine fibre by strainer filtering, pour in higfh-tension ceramics tank afterwards, the boiler flue through dedusting humidification is passed in tank, until pressure reaches 180 ~ 190kPa in higfh-tension ceramics pressure tank table display tank, after keeping stress reaction 12 ~ 18h, make black liquor acidifying; Then open pressure pan pressure-reducing valve, the black liquor after boiler flue gas disposal is moved into bottom with in the aeration tank of aerator, open aeration valve and carry out aeration, at the thick product of aeration tank surface collection lignin; Afterwards thick for lignin product is moved into fermentation tank, inoculate the activated sludge obtained from secondary sedimentation tank of sewage treatment work wherein, activated sludge inoculum concentration is 15 ~ 20% of lignin crude product gross mass, add the thiosulfuric acid sodium crystal of lignin total amount 2 ~ 5% afterwards again, incubator is put into, 40 ~ 50 DEG C of bottom fermentations 4 ~ 5 days after being sealed by fermentation tank mouth preservative film; Subsequently fermentate is moved into beaker, add the absolute ethyl alcohol of fermentate 3 times of volumes, be placed on magnetic stirrer, stir 10 ~ 20min with the rotating speed of 500 ~ 600r/min and obtain mixed liquor, mixed liquor is moved into cloth filter press, press filtration, obtain filtrate, filtrate is moved into water-bath, is warming up to 80 ~ 90 DEG C, pure lignin is separated out in distillation;
The lignin of above-mentioned recovery is put into retort, first be warming up to 70 ~ 80 DEG C with the rate program of 5 DEG C/min, insulation 10 ~ 20min carbonizes in advance, then is warming up to 200 ~ 300 DEG C with the rate program of 8 DEG C/min, insulation charing 40 ~ 60min, obtains carbonized wood quality; Finally by carbonized wood quality obtained above and potash in mass ratio for 3:4 mix after put into mortar and grind, blend after mixing is put into stainless steel tubular reactor, and tubular reactor is put into horizontal tube resistance furnace, by ramp to 80 ~ 90 DEG C of room temperature by 10 DEG C/min, insulation activation 2 ~ 3h, Temperature fall is to room temperature under nitrogen atmosphere again, and whole process nitrogen intake is 80 ~ 100cm
3, namely obtain a kind of lignin high-area carbon catalyst reclaiming lignin and prepare from straw pulp black liquor.
Example 1
First get 3L paper-making black liquid and remove the impurity such as fine fibre by strainer filtering, pour in higfh-tension ceramics tank afterwards, in tank, pass into the boiler flue through dedusting humidification, until pressure reaches 180kPa in higfh-tension ceramics pressure tank table display tank, after keeping stress reaction 12h, make black liquor acidifying; Then open pressure pan pressure-reducing valve, the black liquor after boiler flue gas disposal is moved into bottom with in the aeration tank of aerator, open aeration valve and carry out aeration, at the thick product of aeration tank surface collection lignin; Afterwards thick for lignin product is moved into fermentation tank, inoculate the activated sludge obtained from secondary sedimentation tank of sewage treatment work wherein, activated sludge inoculum concentration is 15% of lignin crude product gross mass, add the thiosulfuric acid sodium crystal of lignin total amount 2% afterwards again, incubator is put into, 40 DEG C of bottom fermentations 4 days after being sealed by fermentation tank mouth preservative film; Subsequently fermentate is moved into beaker, add the absolute ethyl alcohol of fermentate 3 times of volumes, be placed on magnetic stirrer, stir 10min with the rotating speed of 500r/min and obtain mixed liquor, mixed liquor is moved into cloth filter press, press filtration, obtain filtrate, filtrate is moved into water-bath, is warming up to 80 DEG C, pure lignin is separated out in distillation; The lignin of above-mentioned recovery is put into retort, is first warming up to 70 DEG C with the rate program of 5 DEG C/min, insulation 10min carbonizes in advance, then is warming up to 200 DEG C with the rate program of 8 DEG C/min, and insulation charing 40min, obtains carbonized wood quality; Finally by carbonized wood quality obtained above and potash in mass ratio for 3:4 mix after put into mortar and grind, blend after mixing is put into stainless steel tubular reactor, and tubular reactor is put into horizontal tube resistance furnace, by the ramp to 80 DEG C of room temperature by 10 DEG C/min, insulation activation 2h, Temperature fall is to room temperature under nitrogen atmosphere again, and whole process nitrogen intake is 80cm
3, namely obtain a kind of lignin high-area carbon catalyst reclaiming lignin and prepare from straw pulp black liquor.
This example is simple, during use, catalytic lignin agent obtained by the present invention is used in the course of reaction of vegetable oil production biodiesel, wherein, use amount is for adding the catalyst obtained by 5g the present invention in every 3kg reaction bed material oil, finally record, and do not add compared with catalyst that the present invention obtains, the reaction time decreases 20%.
Example 2
First get 3.5L paper-making black liquid and remove the impurity such as fine fibre by strainer filtering, pour in higfh-tension ceramics tank afterwards, in tank, pass into the boiler flue through dedusting humidification, until pressure reaches 185kPa in higfh-tension ceramics pressure tank table display tank, after keeping stress reaction 15h, make black liquor acidifying; Then open pressure pan pressure-reducing valve, the black liquor after boiler flue gas disposal is moved into bottom with in the aeration tank of aerator, open aeration valve and carry out aeration, at the thick product of aeration tank surface collection lignin; Afterwards thick for lignin product is moved into fermentation tank, inoculate the activated sludge obtained from secondary sedimentation tank of sewage treatment work wherein, activated sludge inoculum concentration is 18% of lignin crude product gross mass, add the thiosulfuric acid sodium crystal of lignin total amount 3.5% afterwards again, incubator is put into, 45 DEG C of bottom fermentations 4.5 days after being sealed by fermentation tank mouth preservative film; Subsequently fermentate is moved into beaker, add the absolute ethyl alcohol of fermentate 3 times of volumes, be placed on magnetic stirrer, stir 15min with the rotating speed of 550r/min and obtain mixed liquor, mixed liquor is moved into cloth filter press, press filtration, obtain filtrate, filtrate is moved into water-bath, is warming up to 85 DEG C, pure lignin is separated out in distillation; The lignin of above-mentioned recovery is put into retort, is first warming up to 75 DEG C with the rate program of 5 DEG C/min, insulation 15min carbonizes in advance, then is warming up to 250 DEG C with the rate program of 8 DEG C/min, and insulation charing 50min, obtains carbonized wood quality; Finally by carbonized wood quality obtained above and potash in mass ratio for 3:4 mix after put into mortar and grind, blend after mixing is put into stainless steel tubular reactor, and tubular reactor is put into horizontal tube resistance furnace, by the ramp to 85 DEG C of room temperature by 10 DEG C/min, insulation activation 2.5h, Temperature fall is to room temperature under nitrogen atmosphere again, and whole process nitrogen intake is 90cm
3, namely obtain a kind of lignin high-area carbon catalyst reclaiming lignin and prepare from straw pulp black liquor.
This example is simple, during use, catalytic lignin agent obtained by the present invention is used in the course of reaction of vegetable oil production biodiesel, wherein, use amount is for adding the catalyst obtained by 7g the present invention in every 4kg reaction bed material oil, finally record, and do not add compared with catalyst that the present invention obtains, the reaction time decreases 25%.
Example 3
First get 4L paper-making black liquid and remove the impurity such as fine fibre by strainer filtering, pour in higfh-tension ceramics tank afterwards, in tank, pass into the boiler flue through dedusting humidification, until pressure reaches 190kPa in higfh-tension ceramics pressure tank table display tank, after keeping stress reaction 18h, make black liquor acidifying; Then open pressure pan pressure-reducing valve, the black liquor after boiler flue gas disposal is moved into bottom with in the aeration tank of aerator, open aeration valve and carry out aeration, at the thick product of aeration tank surface collection lignin; Afterwards thick for lignin product is moved into fermentation tank, inoculate the activated sludge obtained from secondary sedimentation tank of sewage treatment work wherein, activated sludge inoculum concentration is 20% of lignin crude product gross mass, add the thiosulfuric acid sodium crystal of lignin total amount 5% afterwards again, incubator is put into, 50 DEG C of bottom fermentations 5 days after being sealed by fermentation tank mouth preservative film; Subsequently fermentate is moved into beaker, add the absolute ethyl alcohol of fermentate 3 times of volumes, be placed on magnetic stirrer, stir 20min with the rotating speed of 600r/min and obtain mixed liquor, mixed liquor is moved into cloth filter press, press filtration, obtain filtrate, filtrate is moved into water-bath, is warming up to 90 DEG C, pure lignin is separated out in distillation; The lignin of above-mentioned recovery is put into retort, is first warming up to 80 DEG C with the rate program of 5 DEG C/min, insulation 20min carbonizes in advance, then is warming up to 300 DEG C with the rate program of 8 DEG C/min, and insulation charing 60min, obtains carbonized wood quality; Finally by carbonized wood quality obtained above and potash in mass ratio for 3:4 mix after put into mortar and grind, blend after mixing is put into stainless steel tubular reactor, and tubular reactor is put into horizontal tube resistance furnace, by the ramp to 90 DEG C of room temperature by 10 DEG C/min, insulation activation 3h, Temperature fall is to room temperature under nitrogen atmosphere again, and whole process nitrogen intake is 100cm
3, namely obtain a kind of lignin high-area carbon catalyst reclaiming lignin and prepare from straw pulp black liquor.
This example is simple, during use, catalytic lignin agent obtained by the present invention is used in the course of reaction of vegetable oil production biodiesel, wherein, use amount is for adding the catalyst obtained by 8g the present invention in every 5kg reaction bed material oil, finally record, and do not add compared with catalyst that the present invention obtains, the reaction time decreases 30%.
Claims (1)
1. from straw pulp black liquor, reclaim the method that lignin prepares lignin high-area carbon catalyst, it is characterized in that concrete preparation process is:
(1) get 3 ~ 4L paper-making black liquid and remove the impurity such as fine fibre by strainer filtering, pour in higfh-tension ceramics tank afterwards, the boiler flue through dedusting humidification is passed in tank, until pressure reaches 180 ~ 190kPa in higfh-tension ceramics pressure tank table display tank, after keeping stress reaction 12 ~ 18h, make black liquor acidifying;
(2) open pressure pan pressure-reducing valve, the black liquor after boiler flue gas disposal is moved into bottom with in the aeration tank of aerator, open aeration valve and carry out aeration, at the thick product of aeration tank surface collection lignin;
(3) thick for lignin product is moved into fermentation tank, inoculate the activated sludge obtained from secondary sedimentation tank of sewage treatment work wherein, activated sludge inoculum concentration is 15 ~ 20% of lignin crude product gross mass, add the thiosulfuric acid sodium crystal of lignin total amount 2 ~ 5% afterwards again, incubator is put into, 40 ~ 50 DEG C of bottom fermentations 4 ~ 5 days after being sealed by fermentation tank mouth preservative film;
(4) fermentate is moved into beaker, add the absolute ethyl alcohol of fermentate 3 times of volumes, be placed on magnetic stirrer, stir 10 ~ 20min with the rotating speed of 500 ~ 600r/min and obtain mixed liquor, mixed liquor is moved into cloth filter press, press filtration, obtain filtrate, filtrate is moved into water-bath, is warming up to 80 ~ 90 DEG C, pure lignin is separated out in distillation;
(5) lignin of above-mentioned recovery is put into retort, first be warming up to 70 ~ 80 DEG C with the rate program of 5 DEG C/min, insulation 10 ~ 20min carbonizes in advance, then is warming up to 200 ~ 300 DEG C with the rate program of 8 DEG C/min, insulation charing 40 ~ 60min, obtains carbonized wood quality;
(6) by carbonized wood quality obtained above and potash in mass ratio for 3:4 mix after put into mortar and grind, blend after mixing is put into stainless steel tubular reactor, and tubular reactor is put into horizontal tube resistance furnace, by ramp to 80 ~ 90 DEG C of room temperature by 10 DEG C/min, insulation activation 2 ~ 3h, Temperature fall is to room temperature under nitrogen atmosphere again, and whole process nitrogen intake is 80 ~ 100cm
3, namely obtain a kind of lignin high-area carbon catalyst reclaiming lignin and prepare from straw pulp black liquor.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109988318A (en) * | 2019-03-27 | 2019-07-09 | 广州市天河区车陂亚贝思烘焙店 | A kind of preparation method of lignin-base fuel thickener |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109988318A (en) * | 2019-03-27 | 2019-07-09 | 广州市天河区车陂亚贝思烘焙店 | A kind of preparation method of lignin-base fuel thickener |
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