CN107558284A - A kind of method that lignin co-production phosphorus potassium complex fertilizer is extracted using fermenting cellulosic ethanol residue as raw material - Google Patents
A kind of method that lignin co-production phosphorus potassium complex fertilizer is extracted using fermenting cellulosic ethanol residue as raw material Download PDFInfo
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- CN107558284A CN107558284A CN201710767980.1A CN201710767980A CN107558284A CN 107558284 A CN107558284 A CN 107558284A CN 201710767980 A CN201710767980 A CN 201710767980A CN 107558284 A CN107558284 A CN 107558284A
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- lignin
- solid
- residue
- fertilizer
- aqueous solution
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Links
- 229920005610 lignin Polymers 0.000 title claims abstract description 125
- 239000003337 fertilizer Substances 0.000 title claims abstract description 77
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 57
- RDXARWSSOJYNLI-UHFFFAOYSA-N [P].[K] Chemical compound [P].[K] RDXARWSSOJYNLI-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 239000002994 raw material Substances 0.000 title claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 44
- 239000003513 alkali Substances 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 39
- 239000007864 aqueous solution Substances 0.000 claims abstract description 37
- 239000000284 extract Substances 0.000 claims abstract description 22
- 238000000926 separation method Methods 0.000 claims abstract description 22
- 238000012545 processing Methods 0.000 claims abstract description 20
- 239000007790 solid phase Substances 0.000 claims abstract description 19
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011591 potassium Substances 0.000 claims abstract description 18
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000002378 acidificating effect Effects 0.000 claims abstract description 11
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 11
- 239000011574 phosphorus Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000000605 extraction Methods 0.000 claims description 19
- 239000010902 straw Substances 0.000 claims description 19
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 16
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 5
- 235000007164 Oryza sativa Nutrition 0.000 claims description 4
- 235000009566 rice Nutrition 0.000 claims description 4
- 241000894006 Bacteria Species 0.000 claims description 3
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims description 3
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims description 3
- 239000011736 potassium bicarbonate Substances 0.000 claims description 3
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 229940005657 pyrophosphoric acid Drugs 0.000 claims description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 2
- 239000002054 inoculum Substances 0.000 claims description 2
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 241000209094 Oryza Species 0.000 claims 2
- 239000010977 jade Substances 0.000 claims 1
- 230000002906 microbiologic effect Effects 0.000 claims 1
- 238000000855 fermentation Methods 0.000 abstract description 17
- 230000004151 fermentation Effects 0.000 abstract description 17
- 239000002956 ash Substances 0.000 description 29
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 21
- 235000019441 ethanol Nutrition 0.000 description 20
- 239000012043 crude product Substances 0.000 description 17
- 229960004756 ethanol Drugs 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 14
- 238000002156 mixing Methods 0.000 description 14
- 150000001875 compounds Chemical class 0.000 description 13
- 238000011084 recovery Methods 0.000 description 13
- 239000002028 Biomass Substances 0.000 description 11
- 241000196324 Embryophyta Species 0.000 description 11
- 240000008042 Zea mays Species 0.000 description 11
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 11
- 239000000835 fiber Substances 0.000 description 10
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 10
- 235000019796 monopotassium phosphate Nutrition 0.000 description 10
- 235000015097 nutrients Nutrition 0.000 description 10
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 10
- 238000001694 spray drying Methods 0.000 description 10
- 239000001913 cellulose Substances 0.000 description 9
- 229920002678 cellulose Polymers 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 8
- 235000005822 corn Nutrition 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 238000013268 sustained release Methods 0.000 description 7
- 239000012730 sustained-release form Substances 0.000 description 7
- 238000001914 filtration Methods 0.000 description 6
- 239000000446 fuel Substances 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 238000003912 environmental pollution Methods 0.000 description 5
- 239000002689 soil Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 235000009973 maize Nutrition 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 2
- 238000005422 blasting Methods 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000002255 enzymatic effect Effects 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- 241000235342 Saccharomycetes Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003225 biodiesel Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000002361 compost Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000008172 hydrogenated vegetable oil Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- Fertilizers (AREA)
Abstract
The invention discloses a kind of method that lignin co-production phosphorus potassium complex fertilizer is extracted using fermenting cellulosic ethanol residue as raw material, comprise the following steps：(1) the alkaline aqueous solution extracting lignin containing potassium element is added into fermentation residue, separation of solid and liquid, obtains solid residue and alkali extract；(2) decomposing agent is added into obtained solid residue and carries out decomposed processing；(3) pH to 2~6 of alkali extract is adjusted with the acidic aqueous solution of phosphorus element-containing, separation of solid and liquid, lignin is produced after the scrubbed drying of solid phase；(4) obtained phosphorus potassium complex fertilizer is dried in filtrate.The present invention adjusts the pH of alkali extract by gradient, the fertilizer efficiency fertilizer efficiency of spacetabs type phosphorus potassium complex fertilizer is controlled, so as to meet the needs of different crops are to phosphorus potassium complex fertilizer.
Description
Technical field
The invention belongs to bioenergy and biological chemical field, and in particular to one kind is using fermenting cellulosic ethanol residue as raw material
The method for extracting lignin co-production phosphorus potassium complex fertilizer.
Background technology
In recent years, petering out and becoming increasingly conspicuous the problems such as environmental pollution with fossil resources such as oil, green is low
The idea of development of carbon deepens continuously the popular feeling, and the refining techniques utilized with biomass full constituent turns into the research that the world has got most of the attention
Development field, wherein alcohol fuel are just progressively permeated in daily life as a kind of reproducible biomass energy.
Global alcohol fuel yield reaches 98,300,000,000 liters within 2015, accounts for total biological liquid fuel (including ethanol, biodiesel
And hydrogenated vegetable oil) yield (about 130,700,000,000 liters) 75%, be the most important liquid recyclable fuel in the whole world, and field of traffic
Generally acknowledged gasoline alternative fuels.So far, alcohol fuel is original mainly with cereal crops, sugar crops and non-grain starch etc.
Material is produced by fermenting, and in order to save food, producing cellulose ethanol as raw material using lignocellulose-like biomass will turn into from now on
Development trend.
At present, cellulose ethanol is integrally still in the commerical test stage, both at home and abroad existing more set demonstration plants.But its with
The cost competitive of grain alcohol is always the commercialized restrictive factor of cellulose ethanol.Lignin as in nature in total amount
On be only second to renewable, the biodegradable natural organic polymer compounds of cellulose, be that uniquely can largely provide can be again
The non-oil resource of raw compound aromatic base, it is to improve biomass resource utilization efficiency to use it to prepare high valuable chemicals
It is crucial.But in actual applications, only very small part lignin is used for other commercial objects, and the overwhelming majority is incinerated
With recovery section heat energy.Therefore, if this partial lignin can be utilized effectively, environmental pollution can not only be mitigated, and one
Determine that the economic benefit that traditional biological is refined can be improved in degree.
Grand nutrition element nitrogen, phosphorus, potassium in soil generally can not meet the needs of plant growth, it is necessary to using it is nitrogenous,
Phosphorus, the chemical fertilizer of potassium are supplied.But because nitrogen easily passes through volatilization, leaching, denitrification loss；Phosphate fertilizer is easy to by soil
A13+、Fe3+And Ca2+、Mg2+It is fixed, form stable precipitation or formed with iron, aluminum oxide and close storage state phosphorus and progressively lose effectively
Property, cause this season utilization rate of chemical fertilizer application very low, therefore, environmental pollution, increasing caused by reduce fertilizer loss, prevent fertilising
Add crop yield, improve utilization rate of fertilizer for the purpose of " efficiently, slow, compound, customizations " developing direction fertilizer development and
Its application technical research, turn into the hot research problem for agricultural economy sustainable development of preserving the ecological environment, promote.The ratio of lignin
Surface area is big, degradable, and humic acid can be generated by microbial degradation in soil, improves soil physico-chemical property, improves soil
Earth permeability, prevents hardened, by the use of lignin as the carrier of fertilizer, absorption, encapsulated fertilizer, can reach the purpose of fertilizer slow release.
In a word, its utilization are both the comprehensive utilization to Liginon Resource in fermenting cellulosic ethanol residue, and solving simultaneously
The loss and pollution of fertilizer, and a kind of new product can be provided to reduce agriculture production cost.
CN200910014038.3 disclose using cotton seed hulls as co-producing cellulose, lignin, composite fertilizer method.Should
Invention changes domestic prior art in water resource waste and environmental pollution the drawbacks of, but its lignin extraction rate is low, wooden
Contain potassium permanganate in quality solution-off agent, it is larger to the destruction of lignin natural structure, and integrated artistic is complicated, cost is higher.
The content of the invention
Goal of the invention：The invention provides one kind lignin co-production phosphorus potassium is extracted by raw material of fermenting cellulosic ethanol residue
The method of composite fertilizer, solve in conventional wooden element production process caused by containing acid or high-salt wastewater, be a kind of economical and save
The lignin separation extracting method of environmental protection.
Technical scheme：One kind of the present invention is extracted lignin co-production phosphorus potassium as raw material using fermenting cellulosic ethanol residue and answered
The method in Hefei, comprises the following steps：
(1) add the alkaline aqueous solution containing potassium element into fermenting cellulosic ethanol residue to be stripped, separation of solid and liquid obtains
Solid residue and alkali extract；
(2) decomposing agent is added in the solid residue obtained to step (1) and carries out decomposed processing；
(3) pH to 2~6 of the alkali extract obtained with the acidic aqueous solution regulating step (1) of phosphorus element-containing, separation of solid and liquid
Solid phase and filtrate are obtained, solid phase is scrubbed to be drying to obtain lignin；
(4) obtained phosphorus potassium complex fertilizer is dried in the filtrate that step (3) obtains.
Fermenting cellulosic ethanol residue described in step (1) includes maize straw, straw or rice straw fermented residue, the fiber
Ethanol fermentation residue is made up of solid content and water, and the content of the water is 45~55wt.%.The solid content refers to the fibre of over dry
Tie up ethanol fermentation residue.Fermenting cellulosic ethanol residue refers to maize straw, straw or straw through steam blasting, enzymatic saccharification, band
The solid residue that slag ferments obtained by with bottom mixture separation of solid and liquid after thick tower rectifying, gained fermenting cellulosic ethanol residue enter immediately
Row alkali density；The alkaline aqueous solution containing potassium element includes KOH, K2CO3、KHCO3Or K2HPO4The aqueous solution；The cellulose ethanol
Water and the alkaline aqueous solution containing potassium element in fermentation residue are mixed to get the mixed liquor that alkali concn is 1~10wt.%；Institute
The solid-to-liquid ratio for stating solid content and mixed liquor is 1kg:4~25L；The extraction temperature be 25~130 DEG C, extraction times be 0.5~
5h。
Decomposing agent described in step (2) is HM straw decomposing inoculants, microorganism decomposition agent or ferment bacterium quick rotting agent, described decomposed
The mass ratio of agent and solid residue is 0.01~1g:1kg, the decomposed temperature are room temperature, and the decomposed time is 7~45 days.
The acidic aqueous solution of phosphorus element-containing described in step (3) is phosphoric acid, pyrophosphoric acid, metaphosphoric acid, phosphoric anhydride, polyphosphoric acids
Or the acid saline solution of phosphoric acid, the acidic aqueous solution concentration are 75~95wt.%.
When the pH of regulation alkali extract in step (3) is 2≤pH≤3, the fertilizer efficiency of phosphorus potassium complex fertilizer is made from step (4)
It was less than or equal to 6 weeks more than or equal to 2 weeks；The pH of regulation alkali extract is 3 ＜ pH≤4 in the step (3), phosphorus made from step (4)
The fertilizer efficiency of K composite fertilizer is to be less than or equal to 14 weeks more than 6 weeks；The pH of regulation alkali extract be 4 ＜ pH≤5 in the step (3), is walked
Suddenly the fertilizer efficiency of phosphorus potassium complex fertilizer made from (4) is to be less than or equal to 23 weeks more than 14 weeks；As the pH of regulation alkali extract in step (3)
For 5 ＜ pH≤6, the fertilizer efficiency of phosphorus potassium complex fertilizer made from step (4) is to be less than 23 weeks more than or equal to 5 weeks.
The equipment that separation of solid and liquid uses described in step (1) and (3) is pressurized screen, acroll press washer, the sleeping spiral shell centrifugation of bipyramid
Machine, disk centrifugal separator or plate and frame filter press.The equipment used is dried described in step (3) and (4) to be industrial drier, spray and do
Dry machine or microwave dryer.
Alkali density step, the pH steps of regulation alkali extract in the present invention, are required for carrying out convention stir so that material
Fully mix.
Beneficial effect：The present invention extracts lignin co-production phosphorus potassium complex fertilizer by raw material of fermenting cellulosic ethanol residue, real
The full constituent for having showed biomass utilizes；By the present invention in that extracting lignin with the alkaline aqueous solution containing potassium, and utilize phosphorous
The pH of acidic aqueous solution regulation alkali extract is 2~6, both ensure that the extracted amount of lignin, and had solved conventional wooden element again and carry
To take can produce in method containing acid or the problem of high-salt wastewater, the co-production spacetabs type phosphorus potassium complex fertilizer of high added value.Due to multiple
Contain a certain amount of lignin in Hefei, improve the utilization rate of phosphorus potassium complex fertilizer and sustainable cycle；When regulation alkali extract
PH be 2≤pH≤3, the fertilizer efficiency of obtained phosphorus potassium complex fertilizer is less than or equal to 6 weeks more than or equal to 2 weeks；When regulation alkali extract
PH be 3 ＜ pH≤4, the fertilizer efficiency of obtained phosphorus potassium complex fertilizer is less than or equal to 14 weeks more than 6 weeks；As the pH of regulation alkali extract
For 4 ＜ pH≤5, the fertilizer efficiency of obtained phosphorus potassium complex fertilizer is to be less than or equal to 23 weeks more than 14 weeks；When the pH of regulation alkali extract is 5
＜ pH≤6, the fertilizer efficiency of obtained phosphorus potassium complex fertilizer are to be less than 23 weeks more than or equal to 5 weeks.The present invention makes full use of cellulose ethanol thick
Residue waste heat after tower rectifying participates in extracting, reduces energy consumption of reaction, improves the economy of reaction；The present invention is carried using alkaline process
Lignin is taken, improves the recovery rate of lignin compared with organic solvent or ion liquid abstraction method, and significantly reduce life
Produce cost.
Brief description of the drawings
Fig. 1 is the two-dimensional nucleus magnetic chart of alkali density lignin；
Fig. 2 is biphosphate potassium content, content of lignin in the pH and phosphorus potassium complex fertilizer of alkali extract and is sustained the cycle
Relation.
Embodiment
The fermenting cellulosic ethanol residue that the embodiment of the present invention uses refers to maize straw steam blasting, enzymatic saccharification, band slag
Solid after fermentation and thick tower rectifying obtained by the mixture separation of solid and liquid of bottom, solid content 52.3wt.%.It is wooden in its over dry material
Lignin content is 62.35wt.%, content of cellulose 9.60wt.%, and silicate content of ashes is 11.53wt.%, saccharomycete
Content is 12.71wt.%, and other soluble impurities are 3.56wt.%, 50~80 DEG C of fermentation residue residual temperature, gained cellulose ethanol
Fermentation residue carries out alkali density immediately.Wt.% is mass fraction in the present invention.
Embodiment 1
Take corn stalk fiber ethanol fermentation residue 1kg to put into 8L retort, and add 2.16wt.% thereto
KOH aqueous solution 5.799L with adjust the final alkali concn of reaction solution (refer to water in corn stalk fiber ethanol fermentation residue and
Be alkali concn in the mixed liquor that the KOH aqueous solution is mixed to get, similarly hereinafter) 2wt.%, final solid-to-liquid ratio (refer to corn stalk fiber second
The solid-to-liquid ratio of over dry material and mixed liquor in alcohol fermentation residue, similarly hereinafter) it is 1kg:12L, after under conditions of 70 DEG C alkaline process take out
Carry lignin 3h.After reaction terminates, separation of solid and liquid is carried out using acroll press washer, by the quality of HM straw decomposings and solid phase residue
Than for 0.1g:1kg mixing carries out the rotten processing of heap 15 days, realizes that the returning to the field of biomass recycles, filtrate is lignin liquor.
85wt.% industrial phosphoric acid is slowly added into lignin liquor, it is 4 to adjust its pH, and during which mixing speed is set
For 500rpm.Lignin liquor is injected into plate-frame filtering device afterwards, again separation of solid and liquid.Through drying and processing after solid phase washing,
Lignin solid powder can be obtained；Liquid phase is then spray-dried, and it is compound that final gains can be used as high-efficiency sustained-release phosphorus potassium
Fertilizer uses.
Obtain lignin crude product 317.4g altogether after treatment, its water content is 9.7wt.%, and lignin purity is
84.5wt.%, residual sugar amount are 2.3wt.%, and silicate ash content is 4.9wt.%, and lignin extraction rate is 74.3%；Sprayed altogether
Dry 275.4g, its residual sugar amount are 4.7wt.%, and silicate ash content is 8.6wt.%, content of lignin 14.8wt.%, phosphoric acid
The content of potassium dihydrogen is 70.3wt.%.
Wherein, lignin water content is dried to the quality of reduction and former gross mass after constant weight for the lignin crude product obtained
Ratio, lignin purity is the percentage of lignin quality and product gross mass in the lignin crude product that obtains, lignin
The percentage for the lignin gross mass that recovery rate contains for theory in lignin quality in the lignin crude product of acquisition and raw material,
Biphosphate potassium content is the ratio of the quality of potassium dihydrogen phosphate and spray drying thing gross mass in the spray drying thing obtained, similarly hereinafter.
Embodiment 2
Take corn stalk fiber ethanol fermentation residue 1kg to put into 8L retort, and add 3.30wt.% thereto
KOH aqueous solution 4.753L using the final alkali concn for adjusting reaction solution be 3wt.%, final solid-to-liquid ratio for 1kg:10L, after 80
Alkaline process extracting lignin 2.5h under conditions of DEG C.After reaction terminates, separation of solid and liquid is carried out using acroll press washer, it is rotten by HM stalks
The ripe and mass ratio of solid phase residue is 0.1g:1kg mixing carries out the rotten processing of heap 15 days, realizes that the returning to the field of biomass recycles, filter
Liquid is lignin liquor.
85wt.% industrial phosphoric acid is slowly added into lignin liquor, it is 4 to adjust its pH, and during which mixing speed is set
For 500rpm.Plate-frame filtering device is injected the mixture into afterwards, again separation of solid and liquid.Through drying and processing after solid phase washing, you can
Obtain lignin solid powder；Liquid phase is then spray-dried, and final gains, which can be used as high-efficiency sustained-release phosphorus potassium complex fertilizer, to be made
With.
Obtain lignin crude product 331.4g altogether after treatment, its water content is 7.2wt.%, and lignin purity is
83.9wt.%, residual sugar amount are 2.6wt.%, and silicate ash content is 5.7wt.%, and lignin extraction rate is 79.1%；Sprayed altogether
Dry 368.5g, its residual sugar amount are 4.3wt.%, and silicate ash content is 8.1wt.%, content of lignin 11.2wt.%, phosphoric acid
The content of potassium dihydrogen is 74.7wt.%.
Embodiment 3
Take corn stalk fiber ethanol fermentation residue 1kg to put into 8L retort, and add 4.45wt.% thereto
KOH aqueous solution 4.230L using the final alkali concn for adjusting reaction solution be 4wt.%, final solid-to-liquid ratio for 1kg:9L, after at 90 DEG C
Under conditions of alkaline process extracting lignin 1h.Reaction terminate after, using acroll press washer carry out separation of solid and liquid, by HM straw decomposings with
The mass ratio of solid phase residue is 0.1g:1kg mixing carries out the rotten processing of heap 15 days, realizes that the returning to the field of biomass recycles, liquid is
For lignin liquor.
85wt.% industrial phosphoric acid is slowly added into lignin liquor, it is 4 to adjust its pH, and during which mixing speed is set
For 500rpm.Plate-frame filtering device is injected the mixture into afterwards, again separation of solid and liquid.Through drying and processing after solid phase washing, you can
Obtain lignin solid powder；Liquid phase is then spray-dried, and final gains, which can be used as high-efficiency sustained-release phosphorus potassium complex fertilizer, to be made
With.
Obtain lignin crude product 340.2g altogether after treatment, its water content is 4.8wt.%, and lignin purity is
82.7wt.%, residual sugar amount are 2.8wt.%, and silicate ash content is 7.3wt.%, and lignin extraction rate is 82.1%；Sprayed altogether
Dry 432.9g, its residual sugar amount are 3.8wt.%, and silicate ash content is 6.7wt.%, content of lignin 9.1wt.%, phosphoric acid
The content of potassium dihydrogen is 75.2wt.%.The present embodiment slow-release compound fertilizer plant recovery of nutrient 74%, 14 weeks sustainable cycles of fertilizer efficiency.
Embodiment 4
Take corn stalk fiber ethanol fermentation residue 1kg to put into 8L retort, and add 5.64wt.% thereto
KOH aqueous solution 3.707L using the final alkali concn for adjusting reaction solution be 5wt.%, final solid-to-liquid ratio for 1kg:8L, after 110
Alkaline process extracting lignin 1.5h under conditions of DEG C.After reaction terminates, separation of solid and liquid is carried out using acroll press washer, it is rotten by HM stalks
The ripe and mass ratio of solid phase residue is 0.1g:1kg mixing carries out the rotten processing of heap 15 days, realizes that the returning to the field of biomass recycles, liquid
Body is lignin liquor.
85wt.% industrial phosphoric acid is slowly added into lignin liquor, it is 4 to adjust its pH, and during which mixing speed is set
For 500rpm.Plate-frame filtering device is injected the mixture into afterwards, again separation of solid and liquid.Through drying and processing after solid phase washing, you can
Obtain lignin solid powder；Liquid phase is then spray-dried, and final gains, which can be used as high-efficiency sustained-release phosphorus potassium complex fertilizer, to be made
With.
Obtain lignin crude product 325.7g altogether after treatment, its water content is 4.3wt.%, and lignin purity is
81.9wt.%, residual sugar amount are 2.4wt.%, and silicate ash content is 4.9wt.%, and lignin extraction rate is 78.3%；Sprayed altogether
Dry 492.5g, its residual sugar amount are 2.4wt.%, and silicate ash content is 5.1wt.%, content of lignin 6.7wt.%, phosphoric acid
The content of potassium dihydrogen is 83.8wt.%.
Embodiment 5
Take corn stalk fiber ethanol fermentation residue 1kg to put into 8L retort, and add 7.08wt.% thereto
KOH aqueous solution 2.661L using the final alkali concn for adjusting reaction solution be 6wt.%, final solid-to-liquid ratio for 1kg:6L, after at 50 DEG C
Under conditions of alkaline process extracting lignin 2h.Reaction terminate after, using acroll press washer carry out separation of solid and liquid, by HM straw decomposings with
The mass ratio of solid phase residue is 0.1g:1kg mixing carries out the rotten processing of heap 15 days, realizes that the returning to the field of biomass recycles, liquid is
For lignin liquor.
85wt.% industrial phosphoric acid is slowly added into lignin liquor, it is 4 to adjust its pH, and during which mixing speed is set
For 500rpm.Plate-frame filtering device is injected the mixture into afterwards, again separation of solid and liquid.Through drying and processing after solid phase washing, you can
Obtain lignin solid powder；Liquid phase is then spray-dried, and final gains, which can be used as high-efficiency sustained-release phosphorus potassium complex fertilizer, to be made
With.
Obtain lignin crude product 309.5g altogether after treatment, its water content is 3.7wt.%, and lignin purity is
80.2wt.%, residual sugar amount are 4.3wt.%, and silicate ash content is 8.6wt.%, and lignin extraction rate is 73.3%；Sprayed altogether
Dry 426.9g, its residual sugar amount are 3.5wt.%, and silicate ash content is 6.3wt.%, content of lignin 4.2wt.%, phosphoric acid
The content of potassium dihydrogen is 84.6wt.%.
Embodiment 6
Using the same identical condition of embodiment 3, except that：The pH for adjusting lignin liquor is 2.Lignin is obtained altogether
Crude product 345.7g, its water content are 4.7wt.%, and lignin purity is 91.2wt.%, and residual sugar amount is 0.9wt.%, silicate
Ash content is 1.7wt.%, and lignin extraction rate is 92.1%；Spray drying thing 467.5g is obtained altogether, and its residual sugar amount is 3.7wt.%, silicon
Hydrochlorate ash content is 7.4wt.%, and content of lignin 3.2wt.%, the content of potassium dihydrogen phosphate is 54.3wt.%.The present embodiment
Slow-release compound fertilizer plant recovery of nutrient is 38%, sustainable 2 weeks of fertilizer efficiency.
Embodiment 7
Using the same identical condition of embodiment 3, except that：The pH for adjusting lignin liquor is 2.5.Obtain altogether wooden
Plain crude product 343.9g, its water content are 5.1wt.%, and lignin purity is 89.4wt.%, and residual sugar amount is 2.5wt.%, silicic acid
Salt ash content is 3.8wt.%, and lignin extraction rate is 89.5%；Spray drying thing 451.7g is obtained altogether, its residual sugar amount is 3.4wt.%,
Silicate ash content is 6.9wt.%, and content of lignin 4.3wt.%, the content of potassium dihydrogen phosphate is 65.4wt.%.This implementation
Example and slow-release compound fertilizer plant recovery of nutrient are 43%, sustainable 4 weeks of fertilizer efficiency.
Embodiment 8
Using the same identical condition of embodiment 3, except that：The pH for adjusting lignin liquor is 3.Lignin is obtained altogether
Crude product 342.1g, its water content are 4.5wt.%, and lignin purity is 87.2wt.%, and residual sugar amount is 2.1wt.%, silicate
Ash content is 4.7wt.%, and lignin extraction rate is 87.4%；Spray drying thing 435.7g is obtained altogether, and its residual sugar amount is 4.3wt.%, silicon
Hydrochlorate ash content is 6.5wt.%, and content of lignin 5.5wt.%, the content of potassium dihydrogen phosphate is 72.5wt.%.The present embodiment
Slow-release compound fertilizer plant recovery of nutrient is 51%, sustainable 6 weeks of fertilizer efficiency.
Embodiment 9
Using the same identical condition of embodiment 3, except that：The pH for adjusting lignin liquor is 3.5.Obtain altogether wooden
Plain crude product 341.3g, its water content are 4.9wt.%, and lignin purity is 85.1wt.%, and residual sugar amount is 2.5wt.%, silicic acid
Salt ash content is 5.3wt.%, and lignin extraction rate is 84.7%；Spray drying thing 439.4g is obtained altogether, its residual sugar amount is 4.5wt.%,
Silicate ash content is 6.1wt.%, and content of lignin 7.9wt.%, the content of potassium dihydrogen phosphate is 76.3wt.%.This implementation
Example sustained release phosphorus potassium complex fertilizer plant recovery of nutrient is 62%, sustainable 10 weeks of fertilizer efficiency.
Embodiment 10
Using the same identical condition of embodiment 3, except that：The pH for adjusting lignin liquor is 4.5.Obtain altogether wooden
Plain crude product 340.7g, its water content are 4.6wt.%, and lignin purity is 81.5wt.%, and residual sugar amount is 5.4wt.%, silicic acid
Salt ash content is 8.6wt.%, and lignin extraction rate is 81.2%；Spray drying thing 426.9g is obtained altogether, its residual sugar amount is 4.7wt.%,
Silicate ash content is 7.2wt.%, and content of lignin 14.3wt.%, the content of potassium dihydrogen phosphate is 74.6wt.%.This implementation
Example slow-release compound fertilizer plant recovery of nutrient is 80%, sustainable 20 weeks of fertilizer efficiency.
Embodiment 11
Using the same identical condition of embodiment 3, except that：The pH for adjusting lignin liquor is 5.Lignin is obtained altogether
Crude product 341.8g, its water content are 5.0wt.%, and lignin purity is 80.7wt.%, and residual sugar amount is 4.6wt.%, silicate
Ash content is 7.3wt.%, and lignin extraction rate is 80.4%；Spray drying thing 432.9g is obtained altogether, and its residual sugar amount is 3.8wt.%, silicon
Hydrochlorate ash content is 6.9wt.%, and content of lignin 19.4wt.%, the content of potassium dihydrogen phosphate is 68.3wt.%.The present embodiment
Slow-release compound fertilizer plant recovery of nutrient is 85%, sustainable 23 weeks of fertilizer efficiency.
Embodiment 12
Using the same identical condition of embodiment 3, except that：The pH for adjusting lignin liquor is 5.5.Obtain altogether wooden
Plain crude product 134.8g, its water content are 5.2wt.%, and lignin purity is 78.6wt.%, and residual sugar amount is 3.4wt.%, silicic acid
Salt ash content is 7.5wt.%, and lignin extraction rate is 30.8%；Spray drying thing 367.3g is obtained altogether, its residual sugar amount is 4.3wt.%,
Silicate ash content is 8.4wt.%, and content of lignin 31.2wt.%, the content of potassium dihydrogen phosphate is 43.7wt.%.This implementation
Example slow-release compound fertilizer plant recovery of nutrient is 89%, sustainable 8 weeks of fertilizer efficiency.
Embodiment 13
Using the same identical condition of embodiment 3, except that：The pH for adjusting lignin liquor is 6.Lignin is obtained altogether
Crude product 79.8g, its water content are 5.5wt.%, and lignin purity is 77.6wt.%, and residual sugar amount is 5.7wt.%, silicate
Ash content is 8.9wt.%, and lignin extraction rate is 17.9%；Spray drying thing 286.7g is obtained altogether, and its residual sugar amount is 4.8wt.%, silicon
Hydrochlorate ash content is 9.2wt.%, and content of lignin 37.8wt.%, the content of potassium dihydrogen phosphate is 23.5wt.%.The present embodiment
Slow-release compound fertilizer plant recovery of nutrient is 93%, sustainable 5 weeks of fertilizer efficiency.
Embodiment 14
Corn stalk fiber ethanol fermentation residue 1000kg is taken to put into 8m3Retort in, and add thereto
For 4.45wt.% KOH aqueous solution 4230L to adjust the final alkali concn of reaction solution as 4wt.%, final solid-to-liquid ratio is 1kg:9L,
The alkaline process extracting lignin 1h under conditions of 90 DEG C.After reaction terminates, separation of solid and liquid is carried out using acroll press washer, by HM straw
Stalk is decomposed and the mass ratio of solid phase residue is 0.1g:1kg mixing carries out the rotten processing of heap 15 days, realizes that the returning to the field of biomass is sharp again
With filtrate is lignin liquor.
85wt.% industrial phosphoric acid is slowly added into lignin liquor, it is 5 to adjust its pH, and during which mixing speed is set
For 500rpm.Plate-frame filtering device is injected the mixture into afterwards, again separation of solid and liquid.Through drying and processing after solid phase washing, you can
Obtain lignin solid powder；Liquid phase is then spray-dried, and final gains, which can be used as high-efficiency sustained-release phosphorus potassium complex fertilizer, to be made
With.
Obtain lignin crude product 341.9kg altogether after treatment, its water content is 4.9wt.%, and lignin purity is
80.3wt.%, residual sugar amount are 3.2wt.%, and silicate ash content is 5.1wt.%, and lignin extraction rate is 80.1%；Sprayed altogether
Dry 452.7kg, its residual sugar amount are 3.2wt.%, and silicate ash content is 5.1wt.%, content of lignin 17.4wt.%, phosphorus
The content of acid dihydride potassium is 72.3wt.%.The present embodiment slow-release compound fertilizer plant recovery of nutrient is 82%, sustainable 21 weeks of fertilizer efficiency.
Fermenting cellulosic ethanol residue is currently used primarily in combustion heat supplying, and early stage need to be through clamp dog, drying and processing, totle drilling cost 100
Yuan/ton, can and other effects replace lignite (400 yuan/ton), but this method fails efficiently to utilize fermentation residue, meeting simultaneously
Produce serious environmental pollution.According to processing 1t fermenting cellulosic ethanols residue carry out cost accounting, it is necessary to processing charges (containing water rate,
The electricity charge, steam etc.) 180 yuan, 2824 yuan of chemicals puts into 3004 yuan altogether, 4477 yuan of product output, while can obtain compost etc.
Addition product, and three wastes produce.Wherein, 0.79 yuan/kilowatt hour of commercial power, 2.1 yuan/m of running water3, heat steam 124
Yuan/ton；8000 yuan/ton of KOH, 4000 yuan/ton of industrial phosphoric acid, 9500 yuan/ton of potassium dihydrogen phosphate, 4000 yuan/ton of rugose wood element.
Embodiment 15
Using the same identical condition of embodiment 3, except that final alkali concn is 1wt.% during alkali density, final solid-liquid
Than for 1kg:4L, the alkaline process extracting lignin 5h under conditions of 130 DEG C.The mass ratio of HM straw decomposings and solid phase residue is
0.01g:1kg mixing carries out the rotten processing of heap 45 days.
Embodiment 16
Using the same identical condition of embodiment 3, except that final alkali concn is 10wt.% during alkali density, it is final solid
Liquor ratio is 1kg:25L, the alkaline process extracting lignin 0.5h under conditions of 25 DEG C.The mass ratio of HM straw decomposings and solid phase residue is
1g:1kg mixing carries out the rotten processing of heap 7 days.
Embodiment 17
Using the same identical condition of embodiment 3, except that alkaline aqueous solution is K2CO3The aqueous solution, acidic aqueous solution are
The pyrophosphoric acid aqueous solution.
Embodiment 18
Using the same identical condition of embodiment 3, except that alkaline aqueous solution is KHCO3The aqueous solution, acidic aqueous solution
For the metaphosphoric acid aqueous solution.
Embodiment 19
Using the same identical condition of embodiment 3, except that alkaline aqueous solution is K2HPO4The aqueous solution, acidic aqueous solution
For the phosphoric anhydride aqueous solution.
Embodiment 20
Using the same identical condition of embodiment 3, except that the fermenting cellulosic ethanol residue used is that straw fermentation is residual
Slag.
Embodiment 21
Using the same identical condition of embodiment 3, except that the fermenting cellulosic ethanol residue used is that rice straw fermented is residual
Slag.
Embodiment 22
Using the same identical condition of embodiment 3, except that the decomposing agent used is microorganism decomposition agent.
Embodiment 23
Using the same identical condition of embodiment 3, except that the decomposing agent used is ferment bacterium quick rotting agent.
Claims (9)
1. a kind of method that lignin co-production phosphorus potassium complex fertilizer is extracted using fermenting cellulosic ethanol residue as raw material, its feature exist
In comprising the following steps：
(1) add the alkaline aqueous solution containing potassium element into fermenting cellulosic ethanol residue to be stripped, separation of solid and liquid obtains solid
Residue and alkali extract；
(2) decomposing agent is added in the solid residue obtained to step (1) and carries out decomposed processing；
(3) pH to 2~6 of the alkali extract obtained with the acidic aqueous solution regulating step (1) of phosphorus element-containing, separation of solid and liquid obtains
Solid phase and filtrate, solid phase is scrubbed to be drying to obtain lignin；
(4) obtained phosphorus potassium complex fertilizer is dried in the filtrate that step (3) obtains.
2. according to the method for claim 1, it is characterised in that fermenting cellulosic ethanol residue described in step (1) includes jade
Rice stalk, straw or rice straw fermented residue, the fermenting cellulosic ethanol residue are made up of solid content and water, and the content of the water is
45~55wt.%.
3. according to the method for claim 1, it is characterised in that the alkaline aqueous solution bag containing potassium element described in step (1)
Include KOH, K2CO3、KHCO3Or K2HPO4The aqueous solution.
4. according to the method for claim 2, it is characterised in that the water described in step (1) in fermenting cellulosic ethanol residue
The mixed liquor that alkali concn is 1~10wt.% is mixed to get with the alkaline aqueous solution containing potassium element.
5. according to the method for claim 4, it is characterised in that the solid-to-liquid ratio of solid content and mixed liquor described in step (1)
For 1kg:4~25L.
6. according to the method for claim 1, it is characterised in that extraction temperature described in step (1) is 25~130 DEG C, is taken out
It is 0.5~5h to carry the time.
7. according to the method for claim 1, it is characterised in that decomposing agent described in step (2) is HM straw decomposing inoculants, micro-
Biological decomposition agent or ferment bacterium quick rotting agent, the mass ratio of the decomposing agent and solid residue is 0.01~1g:1kg, it is described decomposed
Temperature is room temperature, and the decomposed time is 7~45 days.
8. according to the method for claim 1, it is characterised in that the acidic aqueous solution bag of phosphorus element-containing described in step (3)
Include the acid saline solution of phosphoric acid, pyrophosphoric acid, metaphosphoric acid, phosphoric anhydride, polyphosphoric acids or phosphoric acid, the concentration of the acidic aqueous solution
For 75~95wt.%.
9. according to the method for claim 1, it is characterised in that in the step (3) pH of regulation alkali extract for 2≤pH≤
3, the fertilizer efficiency of phosphorus potassium complex fertilizer made from step (4) is to be less than or equal to 6 weeks more than or equal to 2 weeks；When regulation alkali density in step (3)
The pH of liquid is 3 ＜ pH≤4, and the fertilizer efficiency of phosphorus potassium complex fertilizer made from step (4) is to be less than or equal to 14 weeks more than 6 weeks；When step (3)
The pH of middle regulation alkali extract is 4 ＜ pH≤5, and the fertilizer efficiency of phosphorus potassium complex fertilizer made from step (4) is to be less than or equal to more than 14 weeks
23 weeks；When the pH of regulation alkali extract in step (3) is 5 ＜ pH≤6, the fertilizer efficiency of phosphorus potassium complex fertilizer is big made from step (4)
In equal to 5 weeks be less than 23 weeks.
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| US20130167603A1 (en) * | 2011-07-03 | 2013-07-04 | Christopher Francis Bathurst | Methods and systems for processing plants and converting cellulosic residue to crude bio-oils |
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| CN1436895A (en) * | 2002-02-09 | 2003-08-20 | 吴晓丽 | Comprehensive utilization method of pulping potash black liquor in paper-making process |
| CN101148376A (en) * | 2007-08-06 | 2008-03-26 | 西安华恒科技实业有限公司 | Non-pollution slurry preparing method and method for producing organic potassium foliage fertilizer |
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