CN101486739B - Preparation of alkali lignin - Google Patents
Preparation of alkali lignin Download PDFInfo
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- CN101486739B CN101486739B CN2008100138463A CN200810013846A CN101486739B CN 101486739 B CN101486739 B CN 101486739B CN 2008100138463 A CN2008100138463 A CN 2008100138463A CN 200810013846 A CN200810013846 A CN 200810013846A CN 101486739 B CN101486739 B CN 101486739B
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- 229920005610 lignin Polymers 0.000 title claims abstract description 31
- 239000003513 alkali Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 230000000694 effects Effects 0.000 claims description 125
- 239000007788 liquid Substances 0.000 claims description 106
- 238000001704 evaporation Methods 0.000 claims description 53
- 230000008020 evaporation Effects 0.000 claims description 53
- 238000010438 heat treatment Methods 0.000 claims description 39
- 238000007701 flash-distillation Methods 0.000 claims description 31
- 239000007787 solid Substances 0.000 claims description 29
- 239000007921 spray Substances 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 17
- 238000009833 condensation Methods 0.000 claims description 16
- 230000005494 condensation Effects 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- 239000000835 fiber Substances 0.000 claims description 14
- 238000005507 spraying Methods 0.000 claims description 9
- 238000001694 spray drying Methods 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 239000003431 cross linking reagent Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000010902 straw Substances 0.000 description 18
- 239000007789 gas Substances 0.000 description 9
- 239000012071 phase Substances 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 5
- 230000008016 vaporization Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 244000025254 Cannabis sativa Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004537 pulping Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- OMOVVBIIQSXZSZ-UHFFFAOYSA-N [6-(4-acetyloxy-5,9a-dimethyl-2,7-dioxo-4,5a,6,9-tetrahydro-3h-pyrano[3,4-b]oxepin-5-yl)-5-formyloxy-3-(furan-3-yl)-3a-methyl-7-methylidene-1a,2,3,4,5,6-hexahydroindeno[1,7a-b]oxiren-4-yl] 2-hydroxy-3-methylpentanoate Chemical compound CC12C(OC(=O)C(O)C(C)CC)C(OC=O)C(C3(C)C(CC(=O)OC4(C)COC(=O)CC43)OC(C)=O)C(=C)C32OC3CC1C=1C=COC=1 OMOVVBIIQSXZSZ-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002972 pentoses Chemical class 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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Abstract
The invention relates to a preparation method of alkali lignin, which is characterized by small energy consumption and high efficiency. Simultaneously, the alkali lignin prepared with the method is wide-range in application, can be applied as the raw material of a plurality of products with high economic value and can also be applied to preparing excellent water reducing agent. After a small quantity of crosslinking agent is added to, the alkali lignin can be applied to preparing a lignin sand-fixation agent which has good economic benefit.
Description
Technical field
The invention provides a kind of preparation method of alkali lignin, belong to straw pulp black liquor and administer the field.
Background technology
More than 80% grass fiber in China's paper industry raw material.Grass fiber papermaking mainly contains two kinds, alkaline process and sulfite pulping.Alkaline process is to utilize the aqueous solution of alkali electroless medicament to handle plant fiber material, and with the lignin stripping in the raw material, makes fiber from wherein being separated into the method for paper pulp.
After the alkaline process, there are 50% fibrous material and most alkaline matter to be dissolved in the cooking liquor approximately, become black liquor, contain poly-pentose, lignin, sulfate soap and alkaloids in the black liquor waste, so waste water is black.CODcr generally about 100000～180000mg/L, pH value 10～13, CODcr surpasses more than 50 times of emission standard, owing to the decolouring difficulty, enter water body and seriously consume dissolved oxygen, is difficult to handle with general method.
Because mainly containing thing admittedly in the alkaline straw-pulp black liquid is alkali lignin, therefore can be used for producing alkali lignin.The method of producing alkali lignin at present mainly contains following two kinds: a kind of is to add acid or sour gas in the alkaline process black liquor, by the pH that reduces black liquor alkali lignin is separated out, as application number is the Chinese patent of CN95110575.2, comprise the SO2 lignin acidizing separation, among the CaO and causticization regeneration alkali lye, the calcining and decomposing waste residue produces SO2 and produces cement three big steps, application number is the Chinese patent of CN99116492.X, directly add organic polymer ionogen A polyacrylamide in the alkalitropism black liquor, polyacrylate and substitutive derivative etc. thereof, add acidic substance B after the dissolving again, regulate pH value≤5 of black liquor, lignin is assembled immediately, separate out.But mainly there is following some problem in acid-precipitation method: 1. the pH value requires lowly, and it is big to add acid amount, the treatment cost height; 2. the hold-time long, governance efficiency is low; 3. need use the centrifugation of large high-speed whizzer, facility investment is big, the working cost height; 4. the xylogen particle is little, more difficult filtering.
The technology of another kind of preparation alkali lignin is that black liquor vaporizing is concentrated the back spraying drying, it as application number 92103483.0 Chinese patent, it is a kind of method of from black liquid, producing dry powder, particularly from black liquid, produce the method for alkali lignin dry powder, with black liquid directly or be concentrated into to enter again after the 3-30 degree Beaume filters and carry out the high temperature atomizing in the centrifugal atomizer and handle, enter drying in the drying tower afterwards, isolate alkali lignin dry powder by cyclonic separator again.But because alkaline straw-pulp black liquid silicon content height, viscosity is big, and activation energy is very high, and half fiber and heteroproteose cell are many and be easy to rotten and produce precipitation, so power consumption is high during evaporation concentration, and cost is bigger.
The present invention adopts five to imitate the countercurrent evaporation concentration technology, has overcome above-mentioned shortcoming, and energy consumption is few, and steam per ton can be taken away 4-6 ton moisture, and black liquor can be concentrated to the 40-47% non-scaling, and the foul condensate COD of generation is 1500mg/L only, is easy to administer.Simultaneously, the alkali lignin that obtains, of many uses, can be used as multiple raw material with very high economic worth product, also can be used for preparing outstanding water reducer, also can add little amount of crosslinking agent, be used to prepare the xylogen sand-fixation agent, have good economic benefit.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of alkali lignin.
The preparation method of a kind of alkali lignin provided by the invention may further comprise the steps:
(1) evaporation concentration
Adopt five to imitate the countercurrent evaporation concentration technology, alkaline straw-pulp black liquid is imitated from V and is flowed into, heating steam is imitated from I and is flowed into, after alkaline straw-pulp black liquid is imitated heating evaporation through V effect, IV effect, III successively, become low half concentrated black liquid, low half concentrated black liquid becomes half concentrated black liquid after imitating heating evaporation through II effect, I successively, half concentrated black liquid is imitated through II successively again and I is imitated heating evaporation, becomes concentrated black liquid;
(2) drying
By spray granulating or spraying drying, obtain granular or the powdered alkali lignin concentrated black liquid.
After crossing 325 mesh sieves, wherein above-mentioned alkaline straw-pulp black liquid fibre content is not more than 200mg/L, degree Beaume 2-9, solid content=4-15%, pH=9-13, temperature=60-80 ℃.
Described alkaline straw-pulp black liquid carries out flash distillation earlier before flowing into the V effect, preferred flash distillation is carried out 2 times continuously, and the steam that flashes off feeds III respectively and imitates and the IV single-effect evaporator, to make full use of the heat of alkaline straw-pulp black liquid self.
Described five imitate evaporation respectively imitates pressure and be: I is imitated 20-38kPa, and I is imitated 20-38kPa, II imitate-19～0kPa, III imitate-58～-40kPa, IV imitate-73～-60kPa, V effect-84～-79kPa, each imitates pressure is relative barometric point.
Temperature is respectively during each effect of alkaline straw-pulp black liquid process: 100-120 ℃ of I effect, 90-100 ℃ of II effect, 80-90 ℃ of III effect, 70-80 ℃ of IV effect, 57-65 ℃ of V effect.
Degree Beaume was respectively when alkaline straw-pulp black liquid was imitated through each: V is imitated 5-9, IV and is imitated 9-12, III effect 11-14; During for the first time through II effect and I effect, II is imitated 14-17, I and is imitated 18-21; During for the second time through II effect and I effect, II is imitated 23-25, I and is imitated 25-29.
Described low half concentrated black liquid solid content is 20-25%, and degree Beaume is 11-14; Described half concentrated black liquid solid content is 30-35%, and degree Beaume is 18-21, and described concentrated black liquid solid content is 40-47%, and degree Beaume is 25-29.
Described heating steam temperature is 120-200 ℃, and pressure is 0.2-0.4MPa, becomes the cleaning water of condensation through heat exchange after I is imitated inflow, temperature is 105 ℃-120 ℃, preferably described cleaning water of condensation is carried out flash distillation again, the steam that flashes off feeds II and imitates, to improve the heat energy utilization rate.
The spray granulating head temperature is 500～650 ℃ during described spray granulating, 47-70 ℃ of tail temperature, returning charge amount 〉=50%.
The spray-drying tower temperature in is 300-400 ℃ during described spraying drying, temperature out 110-130 ℃.
Below the present invention is launched to describe in detail.
The preparation method of a kind of alkali lignin provided by the invention mainly comprises following two steps:
One, evaporation concentration
The raw material of the inventive method is at the alkaline straw-pulp black liquid from pulp-extruding machine, in order to prevent that subsequent technique is had a negative impact, must earlier black liquor be filtered, to remove Mierocrystalline cellulose wherein, the step of filter fiber is used fibre filter, through the alkaline straw-pulp black liquid fibre content behind the fibre filter (crossing 325 mesh sieve)≤200mg/L, degree Beaume 5-9, solid content=8-15%, pH=9-13, temperature=60-80 ℃.
In order to improve the heat energy utilization rate, the general multiple-effect evaporation that adopts during evaporation concentration, I is imitated and is added heating steam in the multiple-effect evaporation, the secondary steam temperature that wherein steams is lower than heating steam, can be used as that II imitates heating steam, II is imitated the heating steam that the secondary steam that steams is imitated as III, and the like, the heating steam temperature that each is imitated and the working pressure of each effect reduce successively, and each boiling temperature of imitating solution also reduces successively.
Along with the increase of multiple-effect evaporator effect number, the unit steam consumption reduces gradually, but because the multiple-effect evaporator cost is higher, therefore comes from running cost and consider, the present invention adopts five effects to evaporate.
In order to make full use of the heat of black liquor self, improve the heat energy utilization rate, reduce cost, alkaline straw-pulp black liquid can be carried out flash distillation earlier before entering five effect evaporations, preferably carry out 2 flash distillations continuously.Flash distillation makes alkaline straw-pulp black liquid produce small amount of steam, and the III after the steam of 2 flash tanks feeds respectively in the step is imitated and the IV single-effect evaporator, can utilize the heat of alkaline straw-pulp black liquid self.
The temperature that alkaline straw-pulp black liquid flows into flash tank is 60-80 ℃, and after 2 step flash distillations, temperature variation is little, and solid content does not have considerable change, carries out five then and imitates evaporation.
The used equipment of five effect evaporations is quintuple effect evaporator, in the quintuple effect evaporator each is imitated and is divided into three parts usually, can be referring to Fig. 4, topmost is a distribution plate, effect be black liquor evenly distribute that recycle pump is drawn up in each pipe, the centre is an air chamber, heat exchange area for steam and black liquor, this regional evapotranspiration of black liquor concentrates, and foot is a liquid chamber, and the black liquor after the evaporation concentration flows into this position.
Generally speaking, the material in the quintuple effect evaporator can be divided into gas phase and liquid phase two portions, and liquid phase is a black liquor, and gas phase is a steam, flows to as follows respectively:
1, liquid phase is that black liquor flows to: as shown in Figure 2.
2, gas phase is a steam flow: as shown in Figure 3.
Alkaline straw-pulp black liquid flows into the V single-effect evaporator, is concentrated by the steam heating from the IV single-effect evaporator, enters the IV single-effect evaporator, concentrated by the steam heating of imitating, enter low half concentrated black liquid groove, become low half concentrated black liquid from III, solid content is 20-25%, and degree Beaume is 11-14.
Low half concentrated black liquid enters II single-effect evaporator and I single-effect evaporator then successively, is heated by steam to enter half concentrated black liquid groove after concentrating, and becomes half concentrated black liquid, and solid content is 30-35%, and degree Beaume is 18-21.
Half concentrated black liquid enters the II effect again successively and I is imitated the black liquor groove, is heated by steam to concentrate promptly to become concentrated black liquid, flows into the concentrated black liquid groove.
The concentrated black liquid solid content is 40-47%, and degree Beaume is 25-29.
In quintuple effect evaporator, gas phase is that the flow direction of steam is just opposite, and purpose is to increase the temperature head between gas phase and liquid phase, improves heat exchanger effectiveness.Wherein, the initial vapor temperature of coming out from vapour generator is 200-210 ℃, pressure=0.8-1MPa, drop to 0.2-0.4MPa, about 140 ℃ through reducing valve, feeding I imitates, the steam of this moment is cleaning steam, after the black liquor of imitating with I carries out heat exchange, become the cleaning water of condensation, the temperature of cleaning water of condensation is 105 ℃-120 ℃, in order to make full use of its heat, it is passed through a flash tank, the steam of flash distillation feeds the II single-effect evaporator, and the cleaning water of condensation of discharge can be used for the pulp washing of pulping process.
The steam of the black liquor vaporizing that I is imitated enters II and imitates, as the heating steam that II is imitated, same, the evaporated vapor that the steam of the black liquor vaporizing that II is imitated is imitated as III, and the like, the steam of II, III, IV, V black liquor vaporizing is dirty steam, because of it is that last effect boiling black liquor produces, after itself and this effect black liquor carries out heat exchange, promptly form foul condensate, the foul condensate that II, III, IV, V are imitated finally is summarised in together, and COD flows to sewage work and handles about 1500mg/L.
The temperature of black liquor is followed successively by in above-mentioned each effect:
100-120 ℃ of I effect, 90-100 ℃ of II effect, 80-90 ℃ of III effect, 70-80 ℃ of IV effect, V are imitated 57-65 ℃;
Each is imitated black liquid wave hairdressing and is respectively:
Each is imitated black liquid wave hairdressing and is respectively:
V is imitated 5-9, IV and is imitated 9-12, III effect 11-14; During for the first time through II effect and I effect, II is imitated 14-17, I and is imitated 18-21; During for the second time through II effect and I effect, II is imitated 23-25, I and is imitated 25-29.
Each pressure of imitating is:
I effect 20-38kPa, II effect-19～0kPa, III effect-58～-40kPa, IV effect-73～-60kPa, V effect-84～-79kPa, all pressure all are relative pressure in the literary composition, relative normal atmosphere.
Each heat exchange area of imitating can be decided on the designing treatment ability, with the designing treatment ability: and 70 tons/h of vaporize water, handle 2000m every day
3Alkaline straw-pulp black liquid; Logical quantity of steam is 17.5 tons/h under the normal load, and the heat exchange area of every effect is: I is imitated 1600m
2, II imitates 1200m
2, III imitates, IV is imitated, V is imitated all is 900m
2
In addition, in design,, often need N in each single-effect evaporator in order to improve heat exchanger effectiveness
2Remove Deng non-condensable gases, this can realize at air chamber and vacuum pipe junction throttling orifice plate being arranged by connect a vacuum pump at the air chamber place, only allow non-condensable gases to pass through, and water vapour can't pass through.
Two, drying
Alkaline straw-pulp black liquid through concentrating become concentrated black liquid after, with its carry out drying get final product alkali lignin.Come from the consideration of industrialized production, preferred spray granulating of drying means or spraying drying, 500～650 ℃ of spray granulating head temperatures during spray granulating wherein, 47-70 ℃ of tail temperature, returning charge amount 〉=50%.During spraying drying, 300-400 ℃ of spray-drying tower temperature in, temperature out 110-130 ℃, idiographic flow is seen Fig. 5.Concentrated black liquid sprays into the spray tower, and the hot blast that the while roasting kiln provides enters the spray tower, produces pulverous industrial chemicals by dry Sprayable.The tail gas that produces through behind cyclonic separator, blower fan and the wet cleaner, directly be used in the storage tank periphery, as insulation thermal source profit. substantially without any waste gas, waste residue, waste water is discharged. avoid fully surrounding enviroment are produced any pollution.
In a word, technology energy consumption of the present invention is few, adopts modes such as multistep flash distillation and adding throttling orifice plate, to make full use of the heat of steam, steam per ton can be taken away 4-6 ton moisture, and black liquor can be concentrated to the 40-47% non-scaling, the foul condensate COD that produces is 1500mg/L only, is easy to administer.Simultaneously, the alkali lignin that obtains, of many uses, can be used as multiple raw material with very high economic worth product, also can be used for preparing outstanding water reducer, also can add little amount of crosslinking agent, be used to prepare the xylogen sand-fixation agent, have good economic benefit.
Description of drawings
The five effect evaporation technologies that Fig. 1 the present invention adopts
Fig. 2 five is imitated liquid phase flow direction in the evaporation
Fig. 3 five is imitated gas phase flow direction in the evaporation
The brief configuration synoptic diagram of Fig. 4 vaporizer
The spray-drying process of Fig. 5 concentrated black liquid
Embodiment
Embodiment 1
(1) evaporation concentration
Alkaline straw-pulp black liquid fibre content 200mg/L, degree Beaume 2, solid content=4%, pH=9; Temperature is 60 ℃, and straw pulp black liquor is carried out 2 step flash distillations, obtains the straw pulp black liquor after the flash distillation.
Straw pulp black liquor after the flash distillation is carried out five imitate evaporation, five effect evaporative processes are countercurrent multi-effect evaporation, straw pulp black liquor after the flash distillation is imitated from V and is flowed into, heating steam is imitated from I and is flowed into, and the straw pulp black liquor after the flash distillation becomes low half concentrated black liquid after imitating heating evaporation through V effect, IV effect, III successively, after low half concentrated black liquid is imitated heating evaporation through II effect, I successively, become half concentrated black liquid, half concentrated black liquid is imitated through II successively again and I is imitated heating evaporation, becomes concentrated black liquid.
Above-mentioned heating steam temperature is 120 ℃, and pressure is 0.2MPa, becomes the cleaning water of condensation through heat exchange after I is imitated inflow, and temperature is 105 ℃, and described cleaning water of condensation carries out flash distillation again, and the steam that flashes off utilizes once more, to improve the heat energy utilization rate.
Five above-mentioned effect evaporations are respectively imitated pressure and are: I is imitated 20kPa, II effect-19kPa, III effect-58kPa, IV effect-73kPa, V effect-84kPa;
Each imitates black liquor temperature:
100 ℃ of I effects, 90 ℃ of II effects, 80 ℃ of III effects, 70 ℃ of IV effects, V are imitated 57 ℃
: each is imitated black liquid wave hairdressing and is respectively:
V effect 5, IV effect 9, III imitate 11; During for the first time through II effect and I effect, II effect 14, I imitate 18; During for the second time through II effect and I effect, II effect 23, I imitate 25.
Above-mentioned low half concentrated black liquid solid content is 20%, and degree Beaume is 11; Described half concentrated black liquid solid content is 30%, and degree Beaume is 18; Its solid content of the concentrated black liquid that obtains is 40%, and degree Beaume is 25.
(2) spray granulating
Concentrated black liquid is fed the spray granulating machine, 500 ℃ of spray granulating head temperatures, 47 ℃ of tail temperature, returning charge amount 50% obtains granular alkali lignin.
Embodiment 2
(1) evaporation concentration
Alkaline straw-pulp black liquid fibre content 100mg/L, degree Beaume 9, solid content=15%, pH=13
Alkaline straw-pulp black liquid is directly carried out five imitate evaporation, five effect evaporative processes are countercurrent multi-effect evaporation, straw pulp black liquor is imitated from V and is flowed into, heating steam is imitated from I and is flowed into, and straw pulp black liquor becomes low half concentrated black liquid after imitating heating evaporation through V effect, IV effect, III successively, after low half concentrated black liquid is imitated heating evaporation through II effect, I successively, become half concentrated black liquid, half concentrated black liquid is imitated through II successively again and I is imitated heating evaporation, becomes concentrated black liquid.。
Above-mentioned heating steam temperature is 200 ℃, and pressure is 0.4MPa, becomes the cleaning water of condensation through heat exchange after I is imitated inflow, and temperature is 120 ℃.
Five above-mentioned effect evaporations are respectively imitated pressure and are: I is imitated 38kPa, and II is imitated 0kPa, III effect-40kPa, IV effect-60kPa, V effect-79kPa;
Each imitates black liquor temperature:
120 ℃ of I effects, 100 ℃ of II effects, 90 ℃ of III effects, 80 ℃ of IV effects, V are imitated 65 ℃
Each is imitated black liquid wave hairdressing and is respectively:
V effect 9, IV effect 12, III imitate 14; During for the first time through II effect and I effect, II effect 17, I imitate 21; During for the second time through II effect and I effect, II effect 25, I imitate 29.
Above-mentioned low half concentrated black liquid solid content is 25%, and degree Beaume is 14; Described half concentrated black liquid solid content is 35%, and degree Beaume is 21; Its solid content of the concentrated black liquid that obtains is 47%, and degree Beaume is 29.
(2) spray granulating
Concentrated black liquid is fed the spray granulating machine, 650 ℃ of spray granulating head temperatures, 70 ℃ of tail temperature, returning charge amount 70% obtains granular alkali lignin.
Embodiment 3
(1) evaporation concentration
Alkaline straw-pulp black liquid fibre content 50mg/L, degree Beaume 6, solid content=10%, pH=10; Temperature is 70 ℃, and straw pulp black liquor is carried out a step flash distillation, obtains the straw pulp black liquor after the flash distillation.
Straw pulp black liquor after the flash distillation is carried out five imitate evaporation, five effect evaporative processes are countercurrent multi-effect evaporation, straw pulp black liquor after the flash distillation is imitated from V and is flowed into, heating steam is imitated from I and is flowed into, and the straw pulp black liquor after the flash distillation becomes low half concentrated black liquid after imitating heating evaporation through V effect, IV effect, III successively, after low half concentrated black liquid is imitated heating evaporation through II effect, I successively, become half concentrated black liquid, half concentrated black liquid is imitated through II successively again and I is imitated heating evaporation, becomes concentrated black liquid.
Above-mentioned heating steam temperature is 130 ℃, and pressure is 0.3MPa, becomes the cleaning water of condensation through heat exchange after I is imitated inflow, and temperature is 105 ℃, and described cleaning water of condensation carries out flash distillation again, and the steam that flashes off utilizes once more, to improve the heat energy utilization rate.
Above-mentioned heating steam temperature is 140 ℃, and pressure is 0.3MPa, becomes the cleaning water of condensation through heat exchange after I is imitated inflow, and temperature is 110 ℃, and described cleaning water of condensation carries out flash distillation again, and the steam that flashes off utilizes once more, to improve the heat energy utilization rate.
Five above-mentioned effect evaporations are respectively imitated pressure and are: I is imitated 25kPa, II effect-10kPa, III effect-50kPa, IV effect-70kPa, V effect-80kPa;
Each imitates black liquor temperature:
110 ℃ of I effects, 95 ℃ of II effects, 85 ℃ of III effects, 75 ℃ of IV effects, V are imitated 60 ℃
Each is imitated black liquid wave hairdressing and is respectively:
V effect 6, IV effect 10, III imitate 12; During for the first time through II effect and I effect, II effect 15, I imitate 19; During for the second time through II effect and I effect, II effect 24, I imitate 28.
Above-mentioned low half concentrated black liquid solid content is 21%, and degree Beaume is 12; Described half concentrated black liquid solid content is 32%, and degree Beaume is 19; Its solid content of the concentrated black liquid that obtains is 42%, and degree Beaume is 28.
(2) spraying drying
Concentrated black liquid is fed spray-drying tower, 300 ℃ of spray-drying tower temperature ins, 110 ℃ of temperature outs obtain the mealy alkali lignin.
Embodiment 4
(1) evaporation concentration
Alkaline straw-pulp black liquid fibre content 80mg/L, degree Beaume 8, solid content=13%, pH=11; Temperature is 62 ℃, and straw pulp black liquor is carried out 2 step flash distillations, obtains the straw pulp black liquor after the flash distillation.
Straw pulp black liquor after the flash distillation is carried out five imitate evaporation, five effect evaporative processes are countercurrent multi-effect evaporation, straw pulp black liquor after the flash distillation is imitated from V and is flowed into, heating steam is imitated from I and is flowed into, and the straw pulp black liquor after the flash distillation becomes low half concentrated black liquid after imitating heating evaporation through V effect, IV effect, III successively, after low half concentrated black liquid is imitated heating evaporation through II effect, I successively, become half concentrated black liquid, half concentrated black liquid is imitated through II successively again and I is imitated heating evaporation, becomes concentrated black liquid.
Above-mentioned heating steam temperature is 150 ℃, and pressure is 0.35MPa, becomes the cleaning water of condensation through heat exchange after I is imitated inflow, and temperature is 112 ℃, and described cleaning water of condensation carries out flash distillation again, and the steam that flashes off utilizes once more, to improve the heat energy utilization rate.
Five above-mentioned effect evaporations are respectively imitated pressure and are: I is imitated 28kPa, II effect-12kPa, III effect-45kPa, IV effect-65kPa, V effect-82kPa;
Each imitates black liquor temperature:
115 ℃ of I effects, 98 ℃ of II effects, 86 ℃ of III effects, 73 ℃ of IV effects, V are imitated 58 ℃
Each is imitated black liquid wave hairdressing and is respectively:
V effect 8, IV effect 11, III imitate 13; During for the first time through II effect and I effect, II effect 16, I imitate 20; During for the second time through II effect and I effect, II effect 24, I imitate 28.
Above-mentioned low half concentrated black liquid solid content is 22%, and degree Beaume is 13; Described half concentrated black liquid solid content is 33%, and degree Beaume is 20; Its solid content of the concentrated black liquid that obtains is 42%, and degree Beaume is 28.
(2) spraying drying
Concentrated black liquid is fed spray-drying tower, 400 ℃ of spray-drying tower temperature ins, 130 ℃ of temperature outs obtain the mealy alkali lignin.
Claims (10)
1. the preparation method of an alkali lignin is characterized in that, may further comprise the steps:
(1) evaporation concentration
Adopt five to imitate the countercurrent evaporation concentration technology, alkaline straw-pulp black liquid is imitated from V and is flowed into, heating steam is imitated from I and is flowed into, after alkaline straw-pulp black liquid is imitated heating evaporation through V effect, IV effect, III successively, become low half concentrated black liquid, low half concentrated black liquid becomes half concentrated black liquid after imitating heating evaporation through II effect, I successively, half concentrated black liquid is imitated through II successively again and I is imitated heating evaporation, becomes concentrated black liquid; Be not more than 200mg/L after described alkaline straw-pulp black liquid fibre content is crossed 325 mesh sieves, degree Beaume 2-9, solid content are 4-15%, and pH is 9-13, and temperature is 60-80 ℃; Described low half concentrated black liquid solid content is 20-25%, and degree Beaume is 11-14; Described half concentrated black liquid solid content is 30-35%, and degree Beaume is 18-21, and described concentrated black liquid solid content is 40-47%, and degree Beaume is 25-29;
(2) drying
By spray granulating or spraying drying, obtain granular or the powdered alkali lignin concentrated black liquid.
2. preparation method according to claim 1 is characterized in that, described alkaline straw-pulp black liquid carries out flash distillation earlier before flowing into the V effect.
3. preparation method according to claim 2 is characterized in that, described flash distillation is carried out 2 times continuously, and the steam that flashes off feeds III respectively and imitates and the IV single-effect evaporator, to make full use of the heat of alkaline straw-pulp black liquid self.
4. preparation method according to claim 1, it is characterized in that, described five effect evaporations are respectively imitated pressure and are: I is imitated 20-38kPa, I is imitated 20-38kPa, II effect-19～0kPa, III effect-58～-40kPa, IV effect-73～-60kPa, V effect-84～-79kPa, each imitates pressure is relative barometric point.
5. preparation method according to claim 1 is characterized in that, temperature is respectively during each effect of alkaline straw-pulp black liquid process: 100-120 ℃ of I effect, 90-100 ℃ of II effect, 80-90 ℃ of III effect, 70-80 ℃ of IV effect, 57-65 ℃ of V effect.
6. preparation method according to claim 1 is characterized in that, degree Beaume was respectively when alkaline straw-pulp black liquid was imitated through each: V is imitated 5-9, IV and is imitated 9-12, III effect 11-14; During for the first time through II effect and I effect, II is imitated 14-17, I and is imitated 18-21; During for the second time through II effect and I effect, II is imitated 23-25, I and is imitated 25-29.
7. preparation method according to claim 1 is characterized in that, described heating steam temperature is 120-200 ℃, and pressure is 0.2-0.4MPa, becomes the cleaning water of condensation through heat exchange after I is imitated inflow, and temperature is 105 ℃-120 ℃.
8. preparation method according to claim 7 is characterized in that, described cleaning water of condensation is carried out flash distillation again, and the steam that flashes off feeds II and imitates, to improve the heat energy utilization rate.
9. preparation method according to claim 1 is characterized in that, the spray granulating head temperature is 500～650 ℃ during described spray granulating, 47-70 ℃ of tail temperature, returning charge amount 〉=50%.
10. preparation method according to claim 1 is characterized in that, the spray-drying tower temperature in is 300-400 ℃ during described spraying drying, temperature out 110-130 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3516910A (en) * | 1967-05-12 | 1970-06-23 | Grace W R & Co | Removing and inhibiting scale in black liquor evaporators |
| CN1249374A (en) * | 1999-07-15 | 2000-04-05 | 孙连超 | Process for preparing sodium xylose from paper-making black liquor and recovering caustic soda by dry combustion |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3516910A (en) * | 1967-05-12 | 1970-06-23 | Grace W R & Co | Removing and inhibiting scale in black liquor evaporators |
| CN1249374A (en) * | 1999-07-15 | 2000-04-05 | 孙连超 | Process for preparing sodium xylose from paper-making black liquor and recovering caustic soda by dry combustion |
Non-Patent Citations (1)
| Title |
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| 裴保全.麦草浆碱回收的探索.《纸和造纸》.2005,(第5期), * |
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