CN1584201A - Black liquid with washing graded cooking process production in ball and preparing method thereof - Google Patents
Black liquid with washing graded cooking process production in ball and preparing method thereof Download PDFInfo
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- CN1584201A CN1584201A CN 200410056856 CN200410056856A CN1584201A CN 1584201 A CN1584201 A CN 1584201A CN 200410056856 CN200410056856 CN 200410056856 CN 200410056856 A CN200410056856 A CN 200410056856A CN 1584201 A CN1584201 A CN 1584201A
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- 238000010411 cooking Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000005406 washing Methods 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 51
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007787 solid Substances 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 47
- 238000009835 boiling Methods 0.000 claims description 42
- 230000029087 digestion Effects 0.000 claims description 26
- 239000005416 organic matter Substances 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 15
- 244000025254 Cannabis sativa Species 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 10
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 10
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 10
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
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- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 1
- 238000012856 packing Methods 0.000 claims 1
- 238000013022 venting Methods 0.000 claims 1
- 238000004537 pulping Methods 0.000 abstract description 9
- 239000000446 fuel Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000000110 cooling liquid Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 30
- 239000000835 fiber Substances 0.000 description 16
- 229920005610 lignin Polymers 0.000 description 13
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- 235000011121 sodium hydroxide Nutrition 0.000 description 12
- 238000010009 beating Methods 0.000 description 10
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- 238000006073 displacement reaction Methods 0.000 description 8
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- 239000010902 straw Substances 0.000 description 8
- 239000002585 base Substances 0.000 description 6
- 238000007598 dipping method Methods 0.000 description 5
- 229920002472 Starch Polymers 0.000 description 4
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 4
- 150000004056 anthraquinones Chemical class 0.000 description 4
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- YAPQBXQYLJRXSA-UHFFFAOYSA-N theobromine Chemical compound CN1C(=O)NC(=O)C2=C1N=CN2C YAPQBXQYLJRXSA-UHFFFAOYSA-N 0.000 description 4
- 229920002488 Hemicellulose Polymers 0.000 description 3
- 241000209140 Triticum Species 0.000 description 3
- 235000021307 Triticum Nutrition 0.000 description 3
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- 239000002699 waste material Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 235000014633 carbohydrates Nutrition 0.000 description 2
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- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
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Images
Abstract
The invention relates to methods for controlling entire pulping process by controlling black liquid index and black liquid preparation, more concretely, relates to the black liquid with washing graded cooking process production in ball, wherein the black liquid contains residual alkali, solids formed by organics and inorganic, silicon dioxide, inertia oxide. The invention discharges thick black liquid and controls index thereof after the first cooking by the washing graded cooking process, and discharges black liquid and controls index thereof after the second cooking; after the thick black liquid has been evaporated, the product can be directly used as fuel for alkali recover furnace, and the said black liquid can be circularly used in the washing graded cooking process, and serves as raw material for raw material pretreatment and the second cooling liquid.
Description
Technical field
What the present invention relates to is a kind of technology of producing paper pulp with non-wood fibrous raw material, more specifically saying so with fibers in grass class is raw material, with washing fractional digestion technology in the ball, unlike the prior art be that the present invention is a quality index of controlling straw pulp by the process conditions of control index of black liquor and acquisition thereof.
Background technology
In the existing technology boiling, because directly logical Steam Heating, chemical reaction fierceness, i.e. the chemical reaction fierceness of delignification.Not only there is papermaking to starch desired fiber in the raw material, also contains other components of producing the unwanted hemicellulose of paper pulp, lignin and resin, pectin, starch, tannin, pigment, inorganic compound.When boiling, at first under lower temperature, carrying out, just there is lignin to separate with pars fibrosa, when treating that elevated temperature carries out boiling, condensation such as lignin in the low-temp reaction product, poly-pentose etc. again are attached on the surface of fiber, be difficult to again eccysis from the fiber, so lack of homogeneity, the screenings of paper pulp are many, hardness height, the drainability of slurry are poor, need a large amount of water washings to remove the black liquor of heteroproteose cell, hemicellulose, lignin composition, cause the sewage pollution environment, the cost up of more feasible production paper pulp, also giving down, the bleaching in step causes difficulty.1 ton of paper pulp of the every production of this technology of prior art produces the 10-12 ton, even 18 tons of black liquor, and this black liquor viscosity height (generally when concentration 42% 100 be about 460 centipoises when spending).The processing of black liquor is the common technique difficult problem in paper mill, black liquor is directly discharged the severe contamination that causes environment.
Grass class pulping technique is a system engineering, to study the overall process of slurrying according to the inhomogeneity of the biological structure of grass fiber raw material and the particularity of chemical composition, mainly be the characteristics of research fibers in grass class slurrying: 1. heavily get the raw materials ready, silica removal, remove heteroproteose cell, improve pulp quality, drainability reduces the recovery of black liquor; 2. the characteristic of grass fiber delignification.Owing to have more alkali that easy molten lignin is arranged in the grass fiber, its slurrying difficulty is reduced, but it requires higher delignification rate that fiber is dissociated again simultaneously, so its pulping process should be very different with timber.3. owing to silicone content height in the raw material, the carbohydrate content height causes its black liquor viscosity height, and recovery difficult is big.4. grass contains a large amount of heteroproteose cells in now being, papermaking is formed a series of harm.5. the bleachability of straw pulp is good than timber, easily adopts short flow process, and chlorine-free bleaching reaches high whiteness.
There are many technical staff to be devoted to the research of this respect, such as, application number is the processing method of a kind of black liquid of 98111534.9, belong to papermaking waste material processing method field, comprise following processing step: the black liquor after the boiling is entered the black liquor storage pool, during next boiling, after again this black liquor being put into rotary spherical digester, measure the alkalinity of black liquor, the needs according to boiling are added into caustic soda again, carry out boiling.The purpose of this invention is in order to reduce production costs, cut down the consumption of energy, boost productivity, reduce environmental pollution, but this method has just proposed a design, without any technological parameter.
Hubei Polytichnic College's journal 99 years 14 3 phases of volume have been delivered the article that is entitled as " strengthening imagination and Preliminary Practice that dogstail is got the raw materials ready and reforms boiling ", a kind of boiling thinking that this article discloses: low temperature high speed cooking, big liquor ratio boiling, secondary boiling.Comprise hot black liquor preimpregnation (can mend alkali)-pre-steaming-row's black liquor-Bai liquid two steaming-cold spurting particularly.It adopts white liquid displacement carrying out two steamings, then successively with warm black liquor, washings displacement, and has adopted cold spurting.On technology, more complicated, and without any technological parameter.
99 years 3 phases of light industry and machinery have been delivered the article of " the energy saving and pollution alleviation transformation of batch cooking workshop section (author Wang Xiyuan) ", the document is thought on the basis of having summed up RDH (displacement heating fast) technology, boiling of wood pulp Extended Delignification and straw pulp low temperature high speed cooking should possess following condition: warm black liquor, hot black liquor preimpregnation (utilize residual alkali, have dense than low alkali when playing steaming); The bulk delignification initial stage adds white liquid (forming high-alkali, sulphur hydrogen radical ion concentration); Final stage of cooking adopts washing black liquid displacement (reducing stripping lignin intensity and ion concentration); Boiling begins and end has lower temperature; Overall process adopts big liquor ratio, the low even hot digestion of solid content; Cold spurting.The warm black liquor that proposes in pollutant that each section washed out that the document proposes and the pot merges, and reclaims heat and part chemicals then in the preheating preimpregnation, and the document is an imagination, and relevant parameters is not provided.
99 years 4 phases of Jiangsu papermaking disclose one piece and have been entitled as the article of " imagination of rotary spherical digester replacing and digesting technoloy flow process ", and the basic principle of the document is: big liquor ratio (1: 4.5-5); Secondary boiling (indirect temperature black liquor-steaming, hot black liquor displacement two is steamed), displacement washing in the ball, cold spurting, it is dense to replenish alkali with white liquid.The document adopts the outer preimpregnation of white liquid ball, does not disclose concrete technological parameter.
International Paper 20 discloses one piece and has been entitled as the article of " the lab scale research of Trial of Displacement Cooking of Wheat Straw " 1 phases of volume, and this article thinks that the condition of wheat straw alkaline cooking is: the dense uniform distribution in whole digestion process of alkali; Keep the lignin low in the cooking liquor or the concentration of other leachables; Boiling temperature is too not high.The document proposes: carry out white liquid temperature black liquor preimpregnation (being heated to 120 ℃) in the pot, adopt the white liquid and the hot black liquor displacement of different liquor ratios and finish boiling, replace black liquor with washings.
Prior art does not also have the pulping process of the practicable grass fiber of a cover, researcher of the present invention is based on existing ground defective, propose a kind of quality that can not only improve straw pulp, and can reduce the careless class pulping process of the treating capacity and the liquid waste processing difficulty of waste liquid.
Summary of the invention
Main purpose of the present invention is to obtain a kind of black liquor product with brand-new index, can be after the described concentrated black liquid evaporation directly as the alkali recovery furnace fuel applications, the concentrated black liquid product does not contain the straw pulp fiber, the concentration height, but viscosity is low, black liquor is light, there is not precipitation, environmental protection treatment after being convenient to discharge, what is more important, described black liquor can wash continuous recycling in the fractional digestion technology in ball, and as the dogstail pretreatment of raw material with and the raw material of cooking liquor for the second time, further, the present invention passes through the control to the black liquor index, thereby the continuous reuse of black liquor is continued.
Another object of the present invention is to propose a kind of described black liquor technology that obtains, described technology is convenient to separating of fiber and black liquor, and the black liquor viscosity of output is low, solid concentration is high, is convenient to recycle and environmental protection post processing.
Purpose of the present invention can be achieved in the following manner, that is, output concentrated black liquid in the boiling first time, i.e. No. 1 black liquor, output black liquor in the boiling second time, i.e. No. 2 black liquor, the two is all with contained residual alkali, solid content, inorganic matter, organic matter, the ratio of organic matter/inorganic matter, silica characterizes.
Express for clear, (dense) black liquor among the present invention, except indicating clearly that not specified, concentrated black liquid refers to black liquor No. 1 No. 1 No. 2, black liquor refers to black liquor No. 2.
Contain residual alkali 6.5-8.5 grams per liter in said No. 1 black liquor, solid concentration 220-260 grams per liter, inorganic matter is that sulfate ash (in NaOH) is the 85-95 grams per liter, organic matter 145-165 grams per liter, organic matter/inorganic matter 1.55～1.85, silica 6-8.5 grams per liter, total alkali (in sodium oxide molybdena) 50-70 grams per liter, indifferent oxide 0.1～0.3%, said percentage composition are black liquor total solid meter.
Said No. 2 black liquor contain residual alkali 9-11 grams per liter, solid concentration 165-185 grams per liter, inorganic matter sulfate ash (in NaOH) is the 65-75 grams per liter, organic matter 101-131 grams per liter, organic matter/inorganic matter 1.35-1.65, silica 3.5-6.5 grams per liter, total alkali (in sodium oxide molybdena) 40-58 grams per liter, indifferent oxide 0.1-0.3%, said percentage composition are all to black liquor total solid meter.
The PH 11.6-13.0 of said concentrated black liquid (No. 1 black liquor), COD 24-26 ten thousand mg/litre, Baume degrees is 15～18 ° of Be ' (20 ℃); The PH 12.6-13.9 of said black liquor (No. 2 black liquor); COD 15-18.5 ten thousand millis/liter; Baume degrees is 11～14 ° of Be ' (20 ℃).
The manufacture method of black liquor is that black liquor is produced in boiling for the first time No. 1, and black liquor is produced in boiling for the second time No. 2.No. 1 black liquor is as the alkali recovery furnace fuel combustion, No. 2 black liquor as preparation for the first time cooking liquor and for the second time the raw material of cooking liquor recycle.After recycling repeatedly, the concentration of the solid content of black liquor reaches certain value no longer to be increased, and the black liquor of this moment should be discharged.No. 2 black liquor also can be used as fuel.The black liquor viscosity of the inventive method output is low, solid concentration is high.
A kind of method for making with the concentrated black liquid of washing fractional digestion explained hereafter in the ball of the present invention may further comprise the steps:
1) in rotary spherical digester, in rotary spherical digester, adds alkali and the black liquor formation cooking liquor first time after the preliminary treatment, under the rotary spherical digester rotation, in rotary spherical digester, feed steam after needed vapour pressure, carry out little pressure of exitting to rotary spherical digester and approach zero through the grass raw material is carried out;
2) in rotary spherical digester, add again steam make reach desired pressure after, under the rotary spherical digester rotating conditions, be incubated, in requiring the needed time, carry out the cooking reaction first time;
3) for the first time the cooking reaction time arrives, from spurting of rotary spherical digester mouthful take out, discharge opeing, promptly get concentrated black liquid.
Described dipping pretreating process, after comprising in steeper the needed alkali that adds heating and No. 2 black liquor impregnation, under normal pressure, make dipping screw machine rotation 0.1-0.4 hour for well, maceration extract is contacted fully with raw material, make the dipping of raw material evenly complete, can make full use of heat and alkali in the black liquor, with the molten material of the theobromine in the forage, from forage, separate, for boiling provides condition.Behind the dipping, rotary spherical digester with 3-6 rev/min rotating conditions under, normal pressure is in insulation more than 85 degrees centigrade and mix more than 10 minutes, wherein in the insulation of the condition of 85-95 degree with mix 10-40 minute for well.In the alkali that adds in dipping screw machine and rotary spherical digester and No. 2 formed maceration extracts of black liquor, used alkali can be aqueous slkali, for example, NaOH or anthraquinone-NaOH, concentration is 13-15% over dry grass percetage by weight.
The content of alkali is the 25-35 grams per liter in immersion liquid, and over dry material quantity (T) is 1 with the weight ratio of the total liquid measure of maceration extract: 2.1-4.5.
Owing to before the boiling first time, raw material has been carried out preliminary treatment, utilized black liquor as waste material, make black liquor obtain cycling and reutilization, the pressure that black liquor is handled that reduced environment, because to pretreatment of raw material, make at boiling first time heteroproteose cell that time deviates from, hemicellulose, lignin to be that main concentrated black liquid (black liquor) separation is taken out, discharged.
More than alkalinity 26 grams per liters, be good with the 28-32 grams per liter again the first time of adding in rotary spherical digester that alkali and black liquor (No. 2 black liquor) form in the cooking liquor.Over dry material quantity (T) is 1 with the weight ratio of the total liquid measure of the cooking liquor first time: 3.5-5.0.In rotary spherical digester, feed water vapour, make the pressure of steam be 0.3-0.4Mpa after, the pressure to ball of exitting is zero or near zero, again with put to the ball internal pressure be 0-0.02Mpa for well.Under the rotation of rotary spherical digester, make the pressure in the rotary spherical digester reach 0.3-0.4Mpa once more, (be equivalent to about temperature 140 degree) carry out the boiling first time under the pressure condition of 0.3-0.4Mpa, digestion time is 40-80 minute, insulation is 10-40 minute under the pressure of 0.3-0.4Mpa, spurt from rotary spherical digester mouthful take out, discharge opeing, promptly get concentrated black liquid (No. 1 black liquor), then black liquor is detected, with the control indexes of described concentrated black liquid in the preset range that provides.
Because the concentrated black liquid that boiling for the first time produces is taken out, is discharged, fiber in the rotary spherical digester has been carried out the washing of a wet separation matter with regard to being equivalent to cooking liquor for the first time, after carrying out the boiling first time, carry out the boiling second time again again, proceed delignification reaction, so this technology is called washing fractional digestion technology in the ball.After once more little pressure of exitting to rotary spherical digester is reduced to 0.3-0.4MPa, make the pressure of rotary spherical digester rise to 0.6-0.7Mpa (being equivalent to temperature about 155 degree) again, temperature in the ball is risen, under the pressure of 06～0.7Mpa, carry out the boiling second time under the rotary spherical digester rotation, digestion time 40-80 minute, be incubated 20～60 minutes, spurt from rotary spherical digester and mouthful to carry out heat and spurt discharge, carry out countercurrent washing with the traditional wash engine known to the those skilled in the art, form No. 2 black liquor, then described black liquor detected, with the control indexes of described black liquor in the preset range that provides.
When rotary spherical digester rotated, its rotary speed was 3-6 rev/min, with alkali preparation for the first time cooking liquor, used black liquor is black liquor No. 2 during cooking liquor for the second time.
In order to reduce alkaline consumption and to improve the paper pulp rate, in the boiling first time or for the first time, during boiling for the second time, all add a kind of in anthraquinone and the derivative thereof, the addition of anthraquinone and derivative thereof is the 0.6-0.8% of over dry material quantity.Digesting assistant anthraquinone and derivative thereof have the effect that improves delignification and protection carbohydrate.The result of use of anthraquinone is because of the different difference to some extent with pulping process of raw material.
Because after carrying out the boiling first time, the poly-pentose class that is generated in the digestion process, part lignin are discharged for the first time.The pressure ratio of water vapour is lower during boiling for the first time, the temperature in the ball low (about 130 degree).The not condensation of lignin that is generated when making boiling for the first time sticks on the fiber surface, makes the slurry water filtering performance good, and is approaching with wood pulp, residual alkali 0.09-0.2 grams per liter in the slurry.
No. 1 black liquor of after the boiling first time, being produced, one ton of paper pulp is only discharged No. 1 black liquor about 2.7 cubic metres, No. 1 black liquor of one ton of slurry production and the volume of No. 2 black liquor are about 5.7 cubic metres, after adopting technology controlling and process black liquor of the present invention, the pulp quality that its corresponding pulping process is produced is good, can partly replace hardwood pulp.
In the production process of pulp, adopted the technology of washing fractional digestion in the ball, black liquor can repetitive cycling use, and has reduced the pollution to environment, and the black liquor that slurry per ton is discharged can reduce 50%, can save water 50%.And formed paste color is shallow, the whiteness height, hardness is low, intensity folding height, easily making beating, easily bleaching, the physical property performance of comparing its paper pulp with prior art tradition caustic soda AQ technology is respectively: caustic soda AQ technology, thick starch degree K 15.0-18.0, unscreened yield 47.5-50%, screened stock hardness K 10-13, screened stock whiteness (1SO) 36-39%, beating degree 28-32 ° of SR, weight in wet base 2-2.6 gram, fracture length 2-2.8Km, folding strength, 8-15 time, and the thick starch degree of this technology K 9-14, unscreened yield 49.5-52.5%, screened stock hardness K 7-12, screened stock whiteness (1SO) 39-48.7%, beating degree SR 18～28, weight in wet base 4.2-10.2 gram, fracture length 2.7-4.0Km, folding strength 50-150 time (more than be the statistics of 14 rotary spherical digesters).
Its association with pulp bleaching performance is respectively conventional slurry bleaching, hardness k 13.2 before floating, concentration 5.2% before floating, bleaching time 4 hours, bleaching concentration 28g/l, bleachability 7.5%, terminal point whiteness (1SO) 74.5%, the residual chlorine 0.35% of terminal point, 28 ° of SR of beating degree, weight in wet base 1.8g, fracture length 2.875km, folding strength 10 times, hardness k 10.8 before then this technology is floated, concentration 4.3% before floating, bleaching time 4 hours, bleaching concentration 24.7g/l, bleachability 6.7%, terminal point whiteness (1SO) 76.8%, the residual chlorine 0.369/1 of terminal point, 30 ° of SR of beating degree, weight in wet base 2.1 grams, fracture length 3.675km, folding strength 79 times.
35 ° of SR of making beating back paper pulp physical property this technology beating degree, weight in wet base 1.69g, fracture length 3.65km, folding strength 68 times, tearability 480Nm, whiteness (1SO) 76.8%; And 31 ° of SR of conventional boiling beating degree, weight in wet base 1.7g, fracture length 3.254Km, folding strength 26 times, tearability 440Nm, whiteness (1SO) 74.5%.
Black liquor recycles, and no longer increases when the solid concentration of black liquor reaches certain value, and this black liquor should be discharged.
Description of drawings
Fig. 1 is the rotary spherical digester generalized section.
Fig. 2 is a washing fractional digestion process schematic representation in the ball.
1,7 is air inlet pipe among the figure; 2,3 is stop valve; 4 is safety valve; 5 is the worm and gear transmission system; 6 is check (non-return) valve; 8 for spurting bend pipe; 9 for spurting mouth; 10 are the pre-preg processing; 11 is boiling for the first time; 12 is boiling for the second time; 13 are countercurrent washing; No. 1 black liquor of a for discharging; No. 2 black liquor of b for discharging.
The specific embodiment
Below the present invention is further illustrated with specific embodiment, will help the present invention and its advantage of tool are better understood:
Embodiment 1
Present embodiment is described to be, actual pulping process can not obtain two kinds of black liquor of the present invention from beginning, but after technology entered several cycles, the index of two kinds of black liquor began to enter described scope, at this moment, the circulation of described black liquor begins to enter regular.
Therefore, present embodiment is described to be the data that obtain behind process stabilizing, still, and be not precluded within technology and just adopt when initial the black liquor that meets index to handle, for example, the artificial allotment of standard compliant black liquor is with utilization or the like again of the deposit of standard compliant black liquor in the engineering that turned round in the past.
Open in the technology content in front that black liquor described in the present embodiment produces, be not limited to such technology certainly, if the result how other technologies produce in indication range of the present invention, also should be in protection scope of the present invention.After the technology operation is normal, control and contain residual alkali 6.5 grams per liters in described No. 1 black liquor, solid concentration 240 grams per liters, inorganic matter is that sulfate ash (in NaOH) is 85 grams per liters, organic matter 155 grams per liters, organic matter/inorganic matter 1.82, silica 8.5 grams per liters, total alkali (in sodium oxide molybdena) 50 grams per liters, indifferent oxide 0.2%, said percentage composition are black liquor total solid meter.The PH13.0 of said concentrated black liquid (No. 1 black liquor), COD 240,000 mg/litre, Baume degrees ° Be ' is 16.5 (20 ℃);
Then, control described No. 2 black liquor and contain residual alkali 11 grams per liters, solid concentration 201 grams per liters, inorganic matter sulfate ash (in NaOH) is 70 grams per liters, organic matter 131 grams per liters, organic matter/inorganic matter 1.87, silica 5 grams per liters, total alkali (in sodium oxide molybdena) 58 grams per liters, indifferent oxide 0.1%, said percentage composition are all to black liquor total solid meter.The PH12.8 of said black liquor (No. 2 black liquor); COD 18.5 ten thousand millis/liter; Baume degrees is 11 ° of Be ' (20 ℃), and the described controlling index of present embodiment forms complete technical scheme in conjunction with the other technologies content of aforementioned disclosed pulping process.
Other are identical with embodiment 1, different is after the technology operation is normal, controls and contain residual alkali 7 grams per liters in described No. 1 black liquor, solid concentration 235 grams per liters, inorganic matter is that sulfate ash (in NaOH) is 85 grams per liters, organic matter 150 grams per liters, organic matter/inorganic matter 1.76, silica 6 grams per liters, total alkali (in sodium oxide molybdena) 60 grams per liters, indifferent oxide 0.3%, said percentage composition are black liquor total solid meter.The PH11.6 of said concentrated black liquid (No. 1 black liquor), COD 250,000 mg/litre, Baume degrees is 20 ℃ of 18 ° of Be ');
Then, control described No. 2 black liquor and contain residual alkali 9 grams per liters, solid concentration 171 grams per liters, inorganic matter sulfate ash (in NaOH) is 70 grams per liters, organic matter 101 grams per liters, organic matter/inorganic matter 1.44, silica 6.5 grams per liters, total alkali (in sodium oxide molybdena) 40 grams per liters, indifferent oxide 0.2%, said percentage composition are all to black liquor total solid meter.The PH13.9 of said black liquor (No. 2 black liquor); COD 150,000 millis/liter; Baume degrees is 13 ° of Be ' (20 ℃).
Other are identical with embodiment 1, different is after the technology operation is normal, controls and contain residual alkali 8.5 grams per liters in described No. 1 black liquor, solid concentration 255 grams per liters, inorganic matter is that sulfate ash (in NaOH) is 90 grams per liters, organic matter 165 grams per liters, organic matter/inorganic matter 1.83, silica 7 grams per liters, total alkali (in sodium oxide molybdena) 70 grams per liters, indifferent oxide 0.1%, said percentage composition are black liquor total solid meter.The PH 12 of said concentrated black liquid (No. 1 black liquor), COD26 ten thousand mg/litre, Baume degrees is 15 ° of Be ' (20 ℃);
Then, control described No. 2 black liquor and contain residual alkali 10 grams per liters, solid concentration 191 grams per liters, inorganic matter sulfate ash (in NaOH) is 70 grams per liters, organic matter 121 grams per liters, organic matter/inorganic matter 1.72, silica 5 grams per liters, total alkali (in sodium oxide molybdena) 58 grams per liters, indifferent oxide 0.1%, said percentage composition are all to black liquor total solid meter.The PH12.8 of said black liquor (No. 2 black liquor); COD 18.5 ten thousand millis/liter; Baume degrees is 11 ° of Be ' (20 ℃).
Those skilled in the art find by research and a large amount of test, washing fractional digestion technology in the ball that the present invention adopts, can be applied to the slurrying of non-forest fibrous raw material fully, the fibers in grass class raw material carries out delignification under equal condition uniformly, and cooking liquor is in the dense constantly circulation heating down of certain alkali, the lignin of being deviate from is not easy condensation on fiber along with the continuous circulation of cooking liquor adds heat flow, and therefore former pulp brightness can improve 5-8%.The paper pulp that is fit to very much the production soft is also easily bleached and the intensity height.
Washing fractional digestion technology in the described ball, cooking liquor is contacted fully with raw material, the cooking liquor of raw material is mixed fully, can make full use of heat and alkali in the black liquor,, from forage, separate the molten material of the theobromine in the forage, and then through twice boiling, when first time boiling, promptly drive away marrow, the awn of wheat, earth and silicon, and remove whole pentosans and part lignin; When second time boiling, further delignification, the pentosan of oxidation stripping and lignin, good, the easy making beating of the slurry drainability of gained like this, easily bleaching, and also black liquor viscosity is low, the concentration height, and it is easy to extract, recyclable utilization.
The present invention carries out reuse with discharges heat and the chemical agent of boiling effectively, greatly reduces the consumption of the energy, also tool The reduction pulp hardness is arranged, improve pulp quality, reduce alkaline consumption, reduce a series of advantages such as pollution to environment. And And the black liquor control mode that adopts researcher of the present invention to propose, the straw pulp of preparation can the Partial Replacement hardwood pulps, slurry Expect of light color, whiteness is high; Hardness is low, intensity, folding height; Good, the easy making beating of drainability, easily bleaching.
Claims (10)
1. black liquor with washing fractional digestion explained hereafter in the ball, it is characterized in that: be divided into concentrated black liquid and black liquor, the two all characterizes with solid content, silica, the indifferent oxide that residual alkali, organic matter and the inorganic matter that is contained forms.
2. according to the black liquor that washs the fractional digestion explained hereafter in a kind of ball of claim 1, it is characterized in that: contain residual alkali 6.5-8.5 grams per liter in the said concentrated black liquid, solid concentration 220-260 grams per liter, inorganic matter is that sulfate ash (in NaOH) is the 85-95 grams per liter, organic matter is the 145-165 grams per liter, the ratio 1.55～1.85 of organic matter/inorganic matter, silica 6-8.5 grams per liter, total alkali (in sodium oxide molybdena) 50-70 grams per liter, indifferent oxide 0.1～0.3%, said percentage composition are black liquor total solid meter.
3. according to the black liquor that washs the fractional digestion explained hereafter in a kind of ball of claim 1, it is characterized in that: said black liquor contains residual alkali 9-11 grams per liter, solid concentration 165-185 grams per liter, inorganic matter sulfate ash (in NaOH) is the 65-75 grams per liter, organic matter is the 101-131 grams per liter, the ratio 1.35-1.65 of organic matter/inorganic matter, silica 3.5-6.5 grams per liter, total alkali (in sodium oxide molybdena) 40-58 grams per liter, indifferent oxide 0.1-0.3%, said percentage composition are all to black liquor total solid meter.
4. according to the black liquor of washing fractional digestion explained hereafter in claim 1,2 one of them a kind of balls, it is characterized in that, the PH 11.6-13.0 of said concentrated black liquid (No. 1 black liquor), COD 24-26 ten thousand mg/litre, Baume degrees is 15～18 ° of Be ' (20 ℃).
5. according to the black liquor of washing fractional digestion explained hereafter in claim 1,3 one of them a kind of balls, it is characterized in that the PH 12.6-13.9 of said black liquor (No. 2 black liquor); COD 15-18.5 ten thousand millis/liter; Baume degrees is 11～14 ° of Be ' (20 ℃).
6. one kind prepares the described method for making with the black liquor of washing fractional digestion explained hereafter in the ball of claim 1, and the method for making of concentrated black liquid wherein may further comprise the steps:
1) process forms cooking liquor for the first time to add alkali and black liquor after the grass pretreatment of raw material in rotary spherical digester in rotary spherical digester, under the rotary spherical digester rotation, after feeding steam arrives needed vapour pressure in rotary spherical digester, carries out little pressure of exitting to rotary spherical digester and approaches zero;
2) in rotary spherical digester, add again steam make reach desired pressure after, under the rotary spherical digester rotating conditions, be incubated, in requiring the needed time, carry out the cooking reaction first time;
3) for the first time the cooking reaction time arrives, and mouthful carries out pump drainage liquid from spurting of rotary spherical digester, promptly gets concentrated black liquid.
7. the method for making of the black liquor of washing fractional digestion explained hereafter in a kind of ball according to claim 6, it is characterized in that, described pretreatment of raw material is: in the maceration extract that alkali that adds in rotary spherical digester under the condition of normal pressure and black liquor form, used alkali can be aqueous slkali, for NaOH or anthraquinone-naoh concentration are 13-15% over dry grass percetage by weight, the over dry raw material is packed into after preliminary treatment in the rotary spherical digester, under the rotary spherical digester rotating conditions, the raw material of packing in the rotary spherical digester is mixed, under normal pressure in insulation more than 85 degrees centigrade with mix more than 10 minutes.
8. the method for making of the black liquor of washing fractional digestion explained hereafter in a kind of ball according to claim 6, it is characterized in that, the first time of adding in rotary spherical digester that alkali and black liquor form is in the cooking liquor, more than alkalinity 26 grams per liters, be preferably 28～32 grams per liters, the over dry material quantity is 1 with the weight ratio of the total liquid measure of the cooking liquor first time: 3.5-5.0, in rotary spherical digester, feed water vapour, after making the pressure of steam be 0.3-0.4Mpa, the pressure to ball of exitting is zero or near zero, is preferably 0～0.02Mpa; And then in rotary spherical digester, feed steam, and make the pressure in the rotary spherical digester reach 0.3～0.4MPa once more, under the pressure of 0.3～0.4MPa, carry out the boiling first time, digestion time was taken out, is arranged and get black liquor after 40～80 minutes.
9. one kind prepares the described method for making with the black liquor of washing fractional digestion explained hereafter in the ball of claim 1, and the method for making of black liquor wherein may further comprise the steps:
1) in rotary spherical digester, in rotary spherical digester, adds alkali and the black liquor formation cooking liquor first time after the preliminary treatment, under the rotary spherical digester rotation, in rotary spherical digester, feed steam after needed vapour pressure, carry out little pressure of exitting to rotary spherical digester and approach zero through the grass raw material is carried out;
2) in rotary spherical digester, add again steam make reach desired pressure after, under the rotary spherical digester rotating conditions, be incubated, in requiring the needed time, carry out the cooking reaction first time;
3) the cooking reaction time arrives for the first time, takes out, arranges black liquor from the mouth that spurts of rotary spherical digester, is concentrated black liquid;
4) add alkali and black liquor after taking out, discharge concentrated black liquid, form cooking liquor for the second time, in rotary spherical digester, feed steam, make and reach needed vapour pressure in the rotary spherical digester, little venting makes the interior steam drop of rotary spherical digester to needed pressure, adds steam to rotary spherical digester again, reaches required pressure once more;
5) be raised to once more under the pressure that is reached, keeping carrying out heat after the needed time and spurt discharging, washing formed cleaning solution and be called black liquor.
10. the method for making of the black liquor of washing fractional digestion explained hereafter in a kind of ball according to claim 9, it is characterized in that, contain the formed second time more than alkali 16 grams per liters in the cooking liquor, be preferably 16～25 grams per liters, the over dry material quantity is 1 with the weight ratio of total liquid measure of cooking liquor for the second time: 3.5-5.0; Pressure in the rotary spherical digester rises to 0.5～0.6MPa; Once more little pressure of exitting to rotary spherical digester is reduced to 0.3～0.4MPa, makes the pressure in the rotary spherical digester rise to 0.6～0.7Mpa again; Digestion time 40～80 minutes is incubated 20～60 minutes.
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| CNB2004100568567A CN1297708C (en) | 2003-08-26 | 2004-08-25 | Black liquid with washing graded cooking process production in ball and preparing method thereof |
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| CN03156413 | 2003-08-26 | ||
| CN03156413.5 | 2003-08-26 | ||
| CNB2004100568567A CN1297708C (en) | 2003-08-26 | 2004-08-25 | Black liquid with washing graded cooking process production in ball and preparing method thereof |
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| CNB2006101041396A Division CN100489190C (en) | 2004-08-25 | 2004-08-25 | Method for producing black liquid by intraball cleaning stepwise cooking technology |
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| CN1297708C CN1297708C (en) | 2007-01-31 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101451320B (en) * | 2007-12-05 | 2012-05-30 | 山东泉林纸业有限责任公司 | Grass type low brightness pulp, preparation method and use thereof |
| CN112726250A (en) * | 2021-01-11 | 2021-04-30 | 山东晨鸣纸业集团股份有限公司 | Low-solid-content sulfate-method continuous cooking process |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL72750C (en) * | 1947-11-14 | |||
| SE452482B (en) * | 1982-04-28 | 1987-11-30 | Sunds Defibrator | PROCEDURE FOR BATCH PREPARATION OF SULPHATE Pulp WITH HIGH DEGREE |
| US4849052A (en) * | 1983-08-24 | 1989-07-18 | Beloit Corporation | Batch digester multi-stage pulping process |
| SU1498857A1 (en) * | 1987-07-17 | 1989-08-07 | Сибирский научно-исследовательский институт целлюлозы и картона | Method of alkaline digestion of pulp in intermittent-action digesters |
| FI92224C (en) * | 1991-06-28 | 1994-10-10 | Sunds Defibrator Rauma Oy | Batch process for the production of cogeneration |
| FI20001351A0 (en) * | 2000-06-06 | 2000-06-06 | Valmet Chemical Pulping Oy | Eräkeittomenetelmä |
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2004
- 2004-08-25 CN CNB2004100568567A patent/CN1297708C/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101451320B (en) * | 2007-12-05 | 2012-05-30 | 山东泉林纸业有限责任公司 | Grass type low brightness pulp, preparation method and use thereof |
| CN112726250A (en) * | 2021-01-11 | 2021-04-30 | 山东晨鸣纸业集团股份有限公司 | Low-solid-content sulfate-method continuous cooking process |
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