CN101514529A - Method for preparing bamboo dissolving pulp by improved prehydrolysis alkaline process and product thereof - Google Patents
Method for preparing bamboo dissolving pulp by improved prehydrolysis alkaline process and product thereof Download PDFInfo
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Abstract
The invention relates to a method for preparing bamboo dissolving pulp by improved prehydrolysis alkaline process, which comprises the following steps of: bamboo material preparation, in which bamboo is made into bamboo sheets and bamboo threads, the bamboo sheets and threads are washed to remove impurities and dust; pretreatment, which is for removing more organic and nonorganic impurities, and in which the loss of pentosan is less than 2 percent; prehydrolysis, which is carried out at an acid concentration of sulphuric acid and hydrochloric acid of 0.1 to 10.0 weight percent, a temperature of between 80 and 14 DEG C and a liquor ratio of 1:4-15 for 30 to 400 minutes; and alkaline process. The method has the advantages that: the performance index of the bamboo dissolving pulp meets the requirements of viscose fibre pulp and the like; the improved prehydrolysis process allows the major part of pentosan in the bamboo to be hydrolyzed; the hydrolysate can be used as a raw material for xylose, xylitol, L-Arabinitol, ethanol and other products; the improved prehydrolysis process lays a good foundation for cooking and improving the reaction performance of the dissolving pulp; little production cost is added, the treatment load and cost of waste are reduced with the recovery of the products of the prehydrolysis, and the comprehensive cost is the lowest; and the comprehensive utilization of the components of biomass is realized during the pulping process of the dissolving pump.
Description
Technical field
The present invention relates to Chemical Engineering, technology for hydrolyzing, dissolving pulp manufacturing technique field, be specifically related to a kind of improved prehydrolysis alkaline process and make method of bamboo dissolved pulp and products thereof.
Background technology
Lignocellulosic material is mainly used in paper pulp and dissolving pulp, and the latter comprises cellulose viscose pulp, cellulose acetate dissolving pulp, nitrocellulose dissolving pulp and cellulose ether dissolving pulp etc.Cellulose viscose pulp is wherein topmost kind, and cellulose viscose pulp industry has formed complete raw material and technical system through the development of last 100 years.In recent years, along with the rapid expansion of the market demand and fiber production capacity, domestic cellulose viscose pulp consumption also heightens thereupon, needs a large amount of wood pulps of import every year, and the raw material bottleneck is particularly thorny; Simultaneously, along with the growing interest of the whole world to resource and environment, the forest reserves are also precious further.
China's bamboo resource is abundant, and output, kind and cultivated area all account for the world 1/3rd, the more important thing is, bamboo growth period is two to three years, and is short more a lot of than timber, so develop bamboo dissolved pulp the raw material guarantee arranged.The development of dissolving pulp pulping technique has formed sulphite process and alkaline process two big slurrying systems so far, and at the lignocellulosic material of high pentosan content, alkaline process also develops pulping process such as prehydrolysis soda process, prehydrolytic sulfate process.
It is the viscose bamboo pulp manufacture method of feature with the prehydrolysis alkaline process that China Patent No. ZL00135021.8 relates to a kind of, and the prehydrolysis technical conditions are: liquor ratio 1: 2.5～3.5,160～180 ℃ of temperature, are carried out in boiling vessel at 100～180 minutes time.
China Patent No. ZL02112175.3 relates to a kind of method of modifying of insoluble bamboo pulp, promptly papermaking bamboo pulp is further prepared the viscose bamboo pulp with the caustic soda boiling.The method is secondary boiled for raw material, in conjunction with boiling for the first time, and still soda process slurrying in essence, and total processing procedure is long and process repeats, it is serious to change the material waste, and it is big to produce load and carrying capacity of environment, the production cost height.
It is the viscose bamboo pulp manufacture method of feature with the sulphite boiling that China Patent No. ZL02133752.7 relates to a kind of, establishes a pretreatment process before boiling, has been actually the prehydrolysis effect.
Chinese patent publication number CN1970850A relates to a kind of caustic soda pulping process, before boiling, establish a precooking process, its essential is to realize prehydrolysis, when precooking, added a spot of caustic soda, be used for and the prehydrolysis process in organic acids such as the acetic acid that produces and formic acid, alleviate corrosion to digesting apparatus.
Chinese patent publication number CN101158122A relates to a kind of sulfate pulp-making method, has cancelled the prehydrolysis step, and flow process shortens on the surface, but pentosan is all got rid of the wasting of resources as discarded object.
Above-mentioned several public technology that relates to the bamboo dissolved pulp manufacture method in fact still belongs to the traditional alkaline process or the slurrying category of sulphite process.At the high characteristics of bamboo wood pentosan content, the basic technology thought of prehydrolysis is, removes the part pentosan by hydrolysis, and destroys the fibrocyte wall construction, lays the first stone for further removing by boiling.The technique scheme common characteristic is: the so-called no acid hydrolysis of the general employing of the prehydrolysis operation of, setting up before boiling, promptly do not add acid in addition as hydrolyst, but utilize raw material from the acetic acid that when high temperature, decomposites as hydrolyst, the hydrolysing activity of acetic acid has only 1/tens of sulfuric acid and hydrochloric acid, therefore adopt the hydrolysis process of little liquor ratio, high temperature and long-time reaction, prehydrolysis is generally carried out in boiling vessel; Two, the ratio of removing pentosan by prehydrolysis does not have clear and definite control range; Three, to the control of prehydrolysis end product with can stripping and remove and be as the criterion, specifically which kind of product is not controlled, end product is based on furfural generally speaking; Four, the prehydrolysis product is not used substantially, but discarded.
The maximum feature of above-mentioned dissolving pulp pulping process is, be extracted as core with cellulose, with other component in the lignocellulosic material comprise pentosan and lignin as much as possible stripping and separate with cellulose, and get rid of as discarded object usually, embodiment be the thought that the single component of cellulose utilizes in the lignocellulosic material.Here, pentosan hydrolysis and lignin decompose the back as discarded object, from the pulping process angle, produce load and do not reduce, and increased carrying capacity of environment, the waste resource.
In fact, in the bamboo wood except that containing 42～51% cellulose, also contain 19～25% pentosan, be that xylosyl is connected into main chain with (1 → 4) β glycosidic bond, and on the C3 of main chain and C2, be connected with the Arabic glycosyl of L-furans formula, 4-O-methyl-alpha-D-glucose aldehydic acid base or glucuronic acid basal shoot chain.According to string hydrolysis theory, the hydrolysis of these pentosan mainly is divided into two sections, and first section is that pentosan is hydrolyzed to wood sugar and L-arabinose etc., the hydrolysis of so-called polysaccharide just; Second section is that monose such as wood sugar is decomposed into furfural and further decomposes the decomposition of so-called monose just.
In the long duration that plant hydrolyzed industry develops at the beginning of the last century, hemicellulose particularly pentosan is with till hydrolysis and decomposing to furfural, and as industrial chemicals.The prehydrolysis technology of dissolving pulp slurrying is basic synchronous with it at age and technical elements, further decomposes behind the employing pre-hydrolysis method hydrolysis pentosan and removes.In recent years, along with going deep into of natural resources lignocellulosic material application and development,, be that the sugar alcohol industrial development on raw material basis is rapid with the wood sugar as most important pentose, also begin starting by the fermentative Production alcohol fuel.Therefore, the importance and the application prospect of wood sugar highlight, also impel us to examine traditional prehydrolysis alkaline pulping method again closely, propose, the thinking that many components that pentosan is separated too, extracts and uses fully utilize in the cellulosic while of extraction and application.
But up to the present, Shang Weiyou is from lignocellulosic material each component comprehensive utilization thought, most of pentosan in the bamboo wood is hydrolyzed into till the wood sugar and in addition extraction and application and the report of further making bamboo dissolved pulp by alkaline pulping method by control prehydrolysis process.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, but provide a kind of bamboo wood pre-hydrolysis method of control hydrolysis process simultaneously, by regulating hydrolysising condition, the hydrolysis process of control pentosan, suppress the decomposition of monose, the hydrolysis of pentosan is mainly taken place till the wood sugar.
Another technical problem to be solved by this invention is to provide a kind of prepared product of method that adopts improved prehydrolysis alkaline process to make bamboo dissolved pulp, comprises the hydrolyzate and the bamboo dissolved pulp that contain wood sugar.
A technical problem more to be solved by this invention is to provide the purposes of the said goods.
The present invention solves the problems of the technologies described above the technical scheme of being taked: a kind of improved prehydrolysis alkaline process is made the method for bamboo dissolved pulp, comprises the steps:
(1) bamboo wood is got the raw materials ready, and bamboo wood is made bamboo chip or bamboo silk, and impurity and dust are removed in washing;
(2) preliminary treatment is removed more organic and inorganic impurity in the bamboo wood by preliminary treatment, and is made the loss of former relatively bamboo total amount pentosan be less than 2%;
(3) prehydrolysis is carried out in hydrolysis tower or hydrolyzer, and hydrolyst is sulfuric acid or hydrochloric acid, process conditions are: acid concentration is 0.1～10.0wt%, and temperature is 80～140 ℃, and liquor ratio is 1: 4～15, pressure is the saturated vapour pressure under the relevant temperature, and the time is 30～400 minutes;
(4) soda pulping process.
On the basis of such scheme, the bamboo wood that the present invention selects for use is cizu, bambusa textile, west wind bamboo, fishscale bamboo, shank bamboo, presss from both sides one or more mixture in bamboo, green bamboo and the square bamboo in vain.
On the basis of such scheme, step 1 comprises chips and/or tears into bamboo chip or bamboo silk to triennial bamboo wood two, concrete, bamboo wood is cut to the bamboo chip of long 15～30mm, wide 10～20mm, thick 3～8mm by slicer, screen by high frequency shale shaker, and carry out spray washing, removal of contamination and dust with water under high pressure; Or bamboo wood is cut to the bamboo chip that is about 50mm, wide 10～15mm, thickness 3～8mm by slicer, further tear the bamboo silk of the 5～40mm that grows up by the bamboo chip shredder, wherein the bamboo silk of long 20～30mm accounts for more than 70%, bamboo silk distal portion is the wire-dividing broom purification shape, adopt rinsing maching to wash again and carry out dry method and/or wet method of depithing, remove impurity such as most of silt, tabasheer with depithing machine.
Preliminary treatment in above-mentioned steps 2 is to carry out in hydrolysis tower or hydrolyzer, adopts finishing agent to handle, and described finishing agent is sulfuric acid or hydrochloric acid, process conditions are: acid concentration is 0～1.0wt%, temperature is 100～130 ℃, and liquor ratio is 1: 5～15, and the time is 30～180 minutes.
Liquor ratio described in step 2 of the present invention and the step 3 is meant the part by weight of bamboo wood solid content and liquid, is solid-to-liquid ratio.
Concrete, at pretreatment stage, the acid concentration of finishing agent can be 0,0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9 or 1.0wt%, at pretreatment stage, when the finishing agent acid concentration is 0, when promptly not adding finishing agent, only utilize hot water treatment to remove more organic and inorganic impurity;
Treatment temperature can be 100,105,110,115,120,125 or 130 ℃;
Liquor ratio can be 1: 5,1: 6, and 1: 8,1: 10,1: 12,1: 14 or 1: 15;
Time can be 30,50,60,80,100,120,140,160 or 180 minutes.
On the basis of such scheme, in the prehydrolysis of step 3, acid concentration is preferably 0.1～4.0wt%, and the hydrolysis stripping ratio of pentosan is not less than 60% in the former bamboo, and the wood sugar yield of pentosan hydrolysis in the former bamboo is not less than 60%.
Further, the hydrolysis stripping ratio of pentosan is not less than 62% in the former bamboo, as
The hydrolysis stripping ratio of pentosan is not less than 65% in the former bamboo;
The hydrolysis stripping ratio of pentosan is not less than 68% in the former bamboo;
Even the hydrolysis stripping ratio of pentosan is not less than 70% in the former bamboo.
Further, the wood sugar yield of pentosan hydrolysis in the former bamboo is not less than 62%, as
The wood sugar yield of pentosan hydrolysis in the former bamboo is not less than 65%;
The wood sugar yield of pentosan hydrolysis in the former bamboo is not less than 68%;
Even the wood sugar yield of pentosan hydrolysis in the former bamboo is not less than 70%.
Pre-hydrolysis method of the present invention is a kind of method of control hydrolysis process, by the control hydrolysis condition within the specific limits, most of pentosan is hydrolyzed into till the wood sugar, and the least possible pentosan is remained in the bamboo chip or bamboo silk after the hydrolysis, residual ratio is no more than 40%.
According to polysaccharide hydrolysis and monose decomposition kinetics, the speed that polysaccharide hydrolysis and monose decompose is decided by the concentration of acid.In certain acid concentration scope, the maximum output of sugar changes little, and is only relevant with the time, and the concentration of acid doubles, and the time that then reaches peak also shortens half.When being lower than this acid concentration scope, do not follow this rule, and the decomposition rate of sugar is bigger than hydrolysis rate; When being higher than this acid concentration scope, hydrolysis rate increases not obvious, but not sugared organic impurities stripping increases greatly.Therefore the present invention is 0.1～10.0wt% in the acid concentration scope of prehydrolysis stage selection.
Concrete, in the prehydrolysis stage, the acid concentration of hydrolyst can be 0.1,0.2,0.5,0.8,1.0,1.2,1.5,1.8,2.0,2.2,2.5,2.8,3.0,3.2,3.5,3.8,4.0,4.2,4.5,4.8,5.0,5.5,6.0,7.0,8.0,9.0 or 10.0wt%.
Temperature is the potent influence factor of decision hydrolytic process.When temperature improved, the maximum output of monose increased, and simultaneously, the time that reaches peak also significantly shortens, and therefore, the polysaccharide of difficult hydrolysis is hydrolyzed under higher temperature and suits.But the pentosan hydrolysis has its particularity, and pentosan belongs to the facile hydrolysis polysaccharide, and hydrolysis rate is too fast under hot conditions, is difficult to control the formation time of monose maximum output.Therefore prehydrolysis of the present invention is chosen in 80～140 ℃ the lower temperature range and carries out.
Concrete, hydrolysis temperature can be 80,90,100,110,120,130 or 140 ℃.
When liquor ratio within the specific limits the time, sugar yield strengthens along with liquor ratio and increases; When liquor ratio is lower than this scope, it is bigger that the monose productive rate reduces amplitude.When liquor ratio was higher than above-mentioned scope, the monose productive rate increased, but had also reduced the monosaccharide concentration in the hydrolyzate simultaneously, and the following process power consumption will increase, and simultaneously, high liquor ratio has also increased sour consumption.Therefore the present invention's selection is 1: 4～15 with respect to the liquor ratio of dry material.
Concrete, liquor ratio can be 1: 4,1: 5, and 1: 6,1: 8,1: 10,1: 12,1: 14 or 1: 15.
Hydrolysis time depends on the time that is issued to the highest monose productive rate in certain acid concentration, temperature and liquor ratio condition, is generally 30～400 minutes.
Concrete, the time can be 30,60,100,150,200,250,300,350 or 400 minutes.
On the basis of such scheme, the soda pulping process of step 4 is the dissolving pulp pulping process based on soda process or sulfate process, comprises boiling in regular turn, floats preceding selected (purification), bleaches, floats back selected (purification) and the process of manufacturing paper with pulp.This step is to have continued to use technology for many years, will not describe in detail at this.
Wherein, sulfate process is actually the soda process of sulphidity, and the Main Ingredients and Appearance of its cooking liquor is caustic soda and vulcanized sodium, and caustic soda that digestion process consumed and vulcanized sodium can replenish with sodium sulphate.The concrete pulping technique scheme of soda pulping process from boiling to the process of manufacturing paper with pulp all adopts known and disclosed technology.
The invention provides a kind ofly at the prepared product of said method, be the hydrolyzate of getting the raw materials ready through step 1 to 3 bamboo wood, preliminary treatment, prehydrolysis obtain, the main component of hydrolyzate is a reducing sugar, comprises wood sugar, L-arabinose and glucose.Acid in the hydrolyzate comprises as the inorganic acid of hydrolyst and bamboo wood decomposes the organic acid that is produced.Organic matter in the hydrolyzate also comprises nitrogenous thing such as pigment and amino acid and a small amount of monose analyte furfural etc.In addition, also have inorganic matters such as a small amount of ash in the hydrolyzate.By optimizing prehydrolysis technology, can obtain higher reductive hydrolysis sugar yield and hydrolyzate purity and suitable colourity, and minimum pentosan residual rate.In the hydrolyzate, concentration of reduced sugar is 1.5～6.0wt%, and purity is not less than 60%, and the wood sugar ratio is not less than 58% in the reducing sugar, and colourity is moderate.
In the hydrolyzate, concentration of reduced sugar can be the arbitrary concentration among 1.5～6.0wt%, is specifically as follows: 1.5,2.0,2.5,3.0,3.5,4.0,4.5,5.0,5.5 or the 6.0wt% isoconcentration.
Further, hydrolyzate purity can be not less than 65%, as,
Hydrolyzate purity is not less than 70%;
Even hydrolyzate purity is not less than 72%.
The invention provides a kind of purposes at the said hydrolyzed liquid product, further processing and following process to hydrolyzate can adopt known and disclosed technology, as decolouring, depickling, concentrate, purification, ion-exchange, dehydration, hydrogenation are synthetic, biofermentation, chromatography and crystallization etc., further make products such as wood sugar, xylitol, L-arabinose, also can make ethanol and other fermented product by biological fermentation process.
It is a kind of at the prepared product of said method that the present invention provides again, be the bamboo dissolved pulp of getting the raw materials ready through step 1 to 4 bamboo wood, preliminary treatment, prehydrolysis, soda pulping process obtain, by adjusting and control to technological process of whole prehydrolysis soda pulping process and technological parameter, make the every index of bamboo dissolved pulp reach following requirement: dynamic viscosity is 8.28～9.72mPas, alpha cellulose 〉=93.0%, ash≤0.10%, iron part≤20ppm, whiteness 〉=81%, 0.05～3mm
2Little dust≤140mm
2/ Kg oven-dry weight is greater than 3mm
2Big dust≤1.0/Kg oven-dry weight, inhale base number 〉=500%, resin≤0.70%, pentosan≤3.00%, lignin trace, the quantitative 600～800g/m of fourdrinier wire
2, the quantitative 400～600g/m of cylinder
2, delivery moisture content 8.5～11.5%.
The present invention provides a kind of purposes at above-mentioned bamboo dissolved pulp product again, is used for cellulose viscose pulp, cellulose acetate dissolving pulp, nitrocellulose dissolving pulp or cellulose ether dissolving pulp.
The invention has the beneficial effects as follows:
The invention provides a kind of improved prehydrolysis alkaline process and make the method for bamboo dissolved pulp, the bamboo dissolved pulp performance indications reach the requirement of cellulose viscose pulp, cellulose acetate dissolving pulp, nitrocellulose dissolving pulp and cellulose ether dissolving pulp;
By improving prehydrolysis technology, make the pentosan generation hydrolysis of the overwhelming majority in the bamboo wood, obtain reductive hydrolysis sugar concentration, purity and the suitable colourity of zone of reasonableness, can be used as the raw material of products such as wood sugar, xylitol, L-arabinose and ethanol;
Hydrolysising condition of the present invention has also produced maximum destruction to the bamboo fibre cell membrane simultaneously, for boiling and raising dissolving pulp reactivity worth are laid a good foundation;
Owing to only be that prehydrolysis technology before the boiling and equipment are done suitably to adjust, the increase of production cost is very little, the economic benefit of bringing much smaller than the reducing sugar hydrolyzate, in conjunction with the reduction effect of prehydrolysis product recovery, make the comprehensive production cost of hydrolyzate and dissolving pulp minimum to wastewater treatment load and processing cost;
The present invention is from the angle of lignocellulosic material comprehensive utilization, improve traditional prehydrolysis alkaline pulping method and be applied to the bamboo dissolved pulp manufacturing, on engineering, really realized the living beings each component comprehensive utilization of dissolving pulp pulping process first, comprehensive production cost is descended by a relatively large margin, saved resource, and reduced production and carrying capacity of environment to greatest extent, not only economic benefit is considerable, and social benefit is huge.
The specific embodiment
The concrete pulping technique scheme of soda pulping process from boiling to the process of manufacturing paper with pulp all adopts known and disclosed technology in the embodiments of the invention, and, and influence pre-hydrolysis method of the present invention to the general applicability of prehydrolysis alkaline pulping method with constitute the integrality of whole prehydrolysis soda pulping process technical scheme not because of adopting part technological process and the process conditions in certain concrete technical scheme.
Embodiment 1
Provide a kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: two to three years living bamboo woods are cut to the bamboo chip of growing 15～30mm, wide 10～20mm, thick 3～8mm by slicer, screen by high frequency shale shaker, and carry out spray washing with water under high pressure, removal of contamination and dust;
(2) preliminary treatment: carry out in hydrolyzer, finishing agent is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.1wt%, and temperature is 110 ℃, and liquor ratio is 1: 10, in 60 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: carry out in hydrolyzer, hydrolyst is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.7wt%, and temperature is 110 ℃, and liquor ratio is 1: 6, and hydrolysis time 300 minutes adopts Steam Heating, collects hydrolyzate after the hydrolysis, and washes material;
(4) soda pulping process: may further comprise the steps in regular turn:
A, boiling: carry out in boiling vessel, conditions of cooking is: for the oven dry stock amount, be 18～26% in NaOH total alkali consumption, and liquor ratio: 1: 2.0～3.6; Heat up total time: 150～240 minutes, little steam bleeding number of times 〉=2, holding temperature for the first time: 130～150 ℃, temperature retention time: 60～120 minutes, holding temperature for the second time: 155～175 ℃, temperature retention time: 120～240 minutes; Cooking quality is: KMnO
4Value: 4～15, alpha cellulose: 〉=93%, average DP 〉=600;
B, washing;
C, screening: adopt and jump the sieve screening;
D, making beating: light cutter is discongested on beater, requires no little slurry group in the slurry, or is directly spurted by boiling vessel;
E, desanding, concentrate: carry out desanding in desander, technical conditions are: it is dense to remove mortar: 0.7 ± 0.1%, and desanding pressure＞0.28MPa, desanding is starched and densely is: 3.0～3.5% after thickener concentrates;
F, bleaching: adopt the CEH tri-stage bleaching, totally applied chlorine 3.0～4.0%.Chlorination is carried out in the chlorination tower, technical conditions are: chlorination chlorine dosage (for the oven dry stock amount): 1.8～2.8%, account for 60～70% of totally applied chlorine, the chlorination slurry is dense: 3.0～3.5%, time of chlorinating: 40～60 minutes, chlorination temperature: normal temperature, the residual chlorine of chlorination: 〉=0.20g/l, pH value after the chlorination＜2.5 are washed till slurries and are neutral;
Alkalization is carried out in alkalization tower or bleaching machine, and technical conditions are: the alkali refining slurry is dense: 〉=5.0%, and being equivalent to oven dry stock amount alkali charge is 1.5～5.0%, the alkali refining temperature: 50～80 ℃, the alkali refining time: 60～120 minutes, be washed till residual alkali :≤50g/cm
3Bleaching is carried out in bleaching machine, and technical conditions are: the bleaching chlorine dosage: being equivalent to oven dry stock amount chlorine dosage is 0.9～1.6%, accounts for 30～40% of totally applied chlorine, 35～45 ℃ of temperature, bleaching alkalinity :≤250g/cm
3, bleaching time: 120～240 minutes, Bleaching Quality required: whiteness: 〉=75%, and average DP: 〉=450, viscosity: 〉=7.5mPasec, alpha cellulose: 〉=90%, be washed till residual alkali≤50g/cm
3
G, acid treatment, wash material: acid treatment is carried out in bleaching machine, and technical conditions are: be equivalent to the oven dry stock amount, the hydrochloric acid consumption is 2.0～5.0%, the time: 40～60 minutes, and temperature: normal temperature, wash material after the acid treatment, be washed till residual acid :≤0.20g/l;
H, desanding, concentrate, manufacture paper with pulp: carry out desanding in desander, desanding is after thickener makes the dense degree of slurry is 3.0～3.5%; Manufacture paper with pulp on the machine of manufacturing paper with pulp then, technical conditions are: quantitatively 〉=and 400g/m
2, moisture content 8.5～13.0%.
Embodiment 2
Provide another kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 1, two to three years living bamboo woods are cut to the bamboo chip of growing 15～30mm, wide 10～20mm, thick 3～8mm by slicer, screen by high frequency shale shaker, and carry out spray washing with water under high pressure, removal of contamination and dust;
(2) preliminary treatment: with embodiment 1, carry out in hydrolyzer, finishing agent is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.1wt%, and temperature is 110 ℃, and liquor ratio is 1: 10, in 60 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: carry out in hydrolyzer, hydrolyst is a sulfuric acid, and process conditions are: acid concentration is 1.5wt%, and temperature is 125 ℃, and liquor ratio is 1: 10, and hydrolysis time 130 minutes adopts Steam Heating, collects hydrolyzate after the hydrolysis, and washes material;
(4) soda pulping process: with embodiment 1.
Embodiment 3
Provide another improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 1, two to three years living bamboo woods are cut to the bamboo chip of growing 15～30mm, wide 10～20mm, thick 3～8mm by slicer, screen by high frequency shale shaker, and carry out spray washing with water under high pressure, removal of contamination and dust;
(2) preliminary treatment: with embodiment 1, carry out in hydrolyzer, finishing agent is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.1wt%, and temperature is 110 ℃, and liquor ratio is 1: 10, in 60 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: with embodiment 1, carry out in hydrolyzer, hydrolyst is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.7wt%, temperature is 110 ℃, and liquor ratio is 1: 6, hydrolysis time 300 minutes, adopt Steam Heating, collect hydrolyzate after the hydrolysis, and wash material;
(4) soda pulping process: may further comprise the steps in regular turn:
A, boiling: carry out in boiling vessel, conditions of cooking is: for the oven dry stock amount, be 18～26% in NaOH total alkali consumption, and sulphidity: 15～25%, liquor ratio: 1: 2.0～3.6; Heat up total time: 150～240 minutes, little steam bleeding number of times 〉=2, holding temperature for the first time: 130～150 ℃, temperature retention time: 60～120 minutes, holding temperature for the second time: 155～175 ℃, temperature retention time: 120～240 minutes; Batch turning after the boiling, wash material; Cooking quality is: KMnO
4Value: 4～15, alpha cellulose: 〉=93%, average DP 〉=600;
B～H is with embodiment 1.
Embodiment 4
Provide the 4th kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 1, two to three years living bamboo woods are cut to the bamboo chip of growing 15～30mm, wide 10～20mm, thick 3～8mm by slicer, screen by high frequency shale shaker, and carry out spray washing with water under high pressure, removal of contamination and dust;
(2) preliminary treatment: with embodiment 1, carry out in hydrolyzer, finishing agent is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.1wt%, and temperature is 110 ℃, and liquor ratio is 1: 10, in 60 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: with embodiment 2, carry out in hydrolyzer, hydrolyst is a sulfuric acid, and process conditions are: sulfuric acid concentration is 1.5wt%, and temperature is 125 ℃, and liquor ratio is 1: 10, and hydrolysis time 130 minutes adopts Steam Heating.Collect hydrolyzate after the hydrolysis, and wash material;
(4) soda pulping process: with embodiment 3.
Embodiment 5
Provide the 5th kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 1, two to three years living bamboo woods are cut to the bamboo chip of growing 15～30mm, wide 10～20mm, thick 3～8mm by slicer, screen by high frequency shale shaker, and carry out spray washing with water under high pressure, removal of contamination and dust;
(2) preliminary treatment: with embodiment 1, carry out in hydrolyzer, finishing agent is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.1wt%, and temperature is 110 ℃, and liquor ratio is 1: 10, in 60 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: carry out in hydrolyzer, hydrolyst is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.4wt%, and temperature is 110 ℃, and liquor ratio is 1: 6, and hydrolysis time 270 minutes adopts Steam Heating, collects hydrolyzate after the hydrolysis, and washes material;
(4) soda pulping process: with embodiment 1.
Embodiment 6
Provide the 6th kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 1, two to three years living bamboo woods are cut to the bamboo chip of growing 15～30mm, wide 10～20mm, thick 3～8mm by slicer, screen by high frequency shale shaker, and carry out spray washing with water under high pressure, removal of contamination and dust;
(2) preliminary treatment: with embodiment 1, carry out in hydrolyzer, finishing agent is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.1wt%, and temperature is 110 ℃, and liquor ratio is 1: 10, in 60 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: carry out in hydrolyzer, hydrolyst is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.8wt%, and 125 ℃ of temperature, liquor ratio are 1: 10, and hydrolysis time 120 minutes adopts Steam Heating, collects hydrolyzate after the hydrolysis, and washes material;
(4) soda pulping process: with embodiment 1.
Embodiment 7
Provide the 7th kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 1, two to three years living bamboo woods are cut to the bamboo chip of growing 15～30mm, wide 10～20mm, thick 3～8mm by slicer, screen by high frequency shale shaker, and carry out spray washing with water under high pressure, removal of contamination and dust;
(2) preliminary treatment: with embodiment 1, carry out in hydrolyzer, finishing agent is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.1wt%, and temperature is 110 ℃, and liquor ratio is 1: 10, in 60 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: with embodiment 5, carry out in hydrolyzer, hydrolyst is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.4wt%, temperature is 110 ℃, and liquor ratio is 1: 6, hydrolysis time 270 minutes, adopt Steam Heating, collect hydrolyzate after the hydrolysis, and wash material;
(4) soda pulping process: with embodiment 3.
Embodiment 8
Provide the 8th kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 1, two to three years living bamboo woods are cut to the bamboo chip of growing 15～30mm, wide 10～20mm, thick 3～8mm by slicer, screen by high frequency shale shaker, and carry out spray washing with water under high pressure, removal of contamination and dust;
(2) preliminary treatment: with embodiment 1, carry out in hydrolyzer, finishing agent is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.1wt%, and temperature is 110 ℃, and liquor ratio is 1: 10, in 60 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: with embodiment 6, carry out in hydrolyzer, hydrolyst is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.8wt%, and 125 ℃ of temperature, liquor ratio are 1: 10, and hydrolysis time 120 minutes adopts Steam Heating, collects hydrolyzate after the hydrolysis, and washes material;
(4) soda pulping process: with embodiment 3.
Embodiment 9
Provide the 9th kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with two to three years living bamboo woods by slicer be cut to about long 50mm, the bamboo chip of wide 10～15mm, thickness 3～8mm, further by the bamboo chip shredder tear the 5～40mm that grows up, wherein 70% or more for growing the bamboo silk of 20～30mm, distal portion is the wire-dividing broom purification shape, rinsing maching delivered to again by the bamboo silk and the wet method of depithing machine washs and remove marrow, removes impurity such as most of silt, tabasheer;
(2) preliminary treatment: carry out in hydrolyzer, finishing agent is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.1wt%, and temperature is 100 ℃, and liquor ratio is 1: 10, in 50 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: with embodiment 1, carry out in hydrolyzer, hydrolyst is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.7wt%, temperature is 110 ℃, and liquor ratio is 1: 6, hydrolysis time 300 minutes, adopt Steam Heating, collect hydrolyzate after the hydrolysis, and wash material;
(4) soda pulping process: with embodiment 1.
Embodiment 10
Provide the tenth kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 9, with two to three years living bamboo woods by slicer be cut to about long 50mm, the bamboo chip of wide 10～15mm, thickness 3～8mm, further by the bamboo chip shredder tear the 5～40mm that grows up, wherein 70% or more for growing the bamboo silk of 20～30mm, distal portion is the wire-dividing broom purification shape, rinsing maching delivered to again by the bamboo silk and the wet method of depithing machine washs and remove marrow, removes impurity such as most of silt, tabasheer;
(2) preliminary treatment: with embodiment 9, carry out in hydrolyzer, finishing agent is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.1wt%, and temperature is 100 ℃, and liquor ratio is 1: 10, in 50 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: with embodiment 2, carry out in hydrolyzer, hydrolyst is a sulfuric acid, and process conditions are: sulfuric acid concentration is 1.5wt%, temperature is 125 ℃, and liquor ratio is 1: 10, hydrolysis time 130 minutes, adopt Steam Heating, collect hydrolyzate after the hydrolysis, and wash material;
(4) soda pulping process: with embodiment 1.
Embodiment 11
Provide the 11 kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 9, with two to three years living bamboo woods by slicer be cut to about long 50mm, the bamboo chip of wide 10～15mm, thickness 3～8mm, further by the bamboo chip shredder tear the 5～40mm that grows up, wherein 70% or more for growing the bamboo silk of 20～30mm, distal portion is the wire-dividing broom purification shape, rinsing maching delivered to again by the bamboo silk and the wet method of depithing machine washs and remove marrow, removes impurity such as most of silt, tabasheer;
(2) preliminary treatment: with embodiment 9, carry out in hydrolyzer, finishing agent is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.1wt%, and temperature is 100 ℃, and liquor ratio is 1: 10, in 50 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: with embodiment 1, carry out in hydrolyzer, hydrolyst is a sulfuric acid, and process conditions are: sulfuric acid concentration is 0.7wt%, temperature is 110 ℃, and liquor ratio is 1: 6, hydrolysis time 300 minutes, adopt Steam Heating, collect hydrolyzate after the hydrolysis, and wash material;
(4) soda pulping process: with embodiment 3.
Embodiment 12
Provide the 12 kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 9, with two to three years living bamboo woods by slicer be cut to about long 50mm, the bamboo chip of wide 10～15mm, thickness 3～8mm, further by the bamboo chip shredder tear the 5～40mm that grows up, wherein 70% or more for growing the bamboo silk of 20～30mm, distal portion is the wire-dividing broom purification shape, rinsing maching delivered to again by the bamboo silk and the wet method of depithing machine washs and remove marrow, removes impurity such as most of silt, tabasheer;
(2) preliminary treatment: with embodiment 9, carry out in hydrolyzer, finishing agent is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.1wt%, and temperature is 100 ℃, and liquor ratio is 1: 10,50 minutes processing times.In hydrolysis tower or hydrolyzer, carry out, discharge treatment fluid after the preliminary treatment, and wash material;
(3) prehydrolysis: with embodiment 2, carry out in hydrolyzer, hydrolyst is a sulfuric acid, and process conditions are: sulfuric acid concentration is 1.5wt%, temperature is 125 ℃, and liquor ratio is 1: 10, hydrolysis time 130 minutes, adopt Steam Heating, collect hydrolyzate after the hydrolysis, and wash material;
(4) soda pulping process: with embodiment 3.
Embodiment 13
Provide the 13 kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 9, with two to three years living bamboo woods by slicer be cut to about long 50mm, the bamboo chip of wide 10～15mm, thickness 3～8mm, further by the bamboo chip shredder tear the 5～40mm that grows up, wherein 70% or more for growing the bamboo silk of 20～30mm, distal portion is the wire-dividing broom purification shape, rinsing maching delivered to again by the bamboo silk and the wet method of depithing machine washs and remove marrow, removes impurity such as most of silt, tabasheer;
(2) preliminary treatment: with embodiment 9, carry out in hydrolyzer, finishing agent is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.1wt%, and temperature is 100 ℃, and liquor ratio is 1: 10,50 minutes processing times.In hydrolysis tower or hydrolyzer, carry out, discharge treatment fluid after the preliminary treatment, and wash material;
(3) prehydrolysis: with embodiment 5, carry out in hydrolyzer, hydrolyst is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.4wt%, temperature is 110 ℃, and liquor ratio is 1: 6, hydrolysis time 270 minutes, adopt Steam Heating, collect hydrolyzate after the hydrolysis, and wash material;
(4) soda pulping process: with embodiment 1.
Embodiment 14
Provide the 14 kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 9, with two to three years living bamboo woods by slicer be cut to about long 50mm, the bamboo chip of wide 10～15mm, thickness 3～8mm, further by the bamboo chip shredder tear the 5～40mm that grows up, wherein 70% or more for growing the bamboo silk of 20～30mm, distal portion is the wire-dividing broom purification shape, rinsing maching delivered to again by the bamboo silk and the wet method of depithing machine washs and remove marrow, removes impurity such as most of silt, tabasheer;
(2) preliminary treatment: with embodiment 9, carry out in hydrolyzer, finishing agent is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.1wt%, and temperature is 100 ℃, and liquor ratio is 1: 10, in 50 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: with embodiment 6, carry out in hydrolyzer, hydrolyst is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.8wt%, and 125 ℃ of temperature, liquor ratio are 1: 10, and hydrolysis time 120 minutes adopts Steam Heating, collects hydrolyzate after the hydrolysis, and washes material;
(4) soda pulping process: with embodiment 1.
Embodiment 15
Provide the 15 kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 9, with two to three years living bamboo woods by slicer be cut to about long 50mm, the bamboo chip of wide 10～15mm, thickness 3～8mm, further by the bamboo chip shredder tear the 5～40mm that grows up, wherein 70% or more for growing the bamboo silk of 20～30mm, distal portion is the wire-dividing broom purification shape, rinsing maching delivered to again by the bamboo silk and the wet method of depithing machine washs and remove marrow, removes impurity such as most of silt, tabasheer;
(2) preliminary treatment: with embodiment 9, carry out in hydrolyzer, finishing agent is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.1wt%, and temperature is 100 ℃, and liquor ratio is 1: 10, in 50 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: with embodiment 5, carry out in hydrolyzer, hydrolyst is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.4wt%, temperature is 110 ℃, and liquor ratio is 1: 6, hydrolysis time 270 minutes, adopt Steam Heating, collect hydrolyzate after the hydrolysis, and wash material;
(4) soda pulping process: with embodiment 3.
Embodiment 16
Provide the 16 kind of improved prehydrolysis alkaline process to make the method for bamboo dissolved pulp, comprise the steps:
(1) bamboo wood is got the raw materials ready: with embodiment 9, with two to three years living bamboo woods by slicer be cut to about long 50mm, the bamboo chip of wide 10～15mm, thickness 3～8mm, further by the bamboo chip shredder tear the 5～40mm that grows up, wherein 70% or more for growing the bamboo silk of 20～30mm, distal portion is the wire-dividing broom purification shape, rinsing maching delivered to again by the bamboo silk and the wet method of depithing machine washs and remove marrow, removes impurity such as most of silt, tabasheer;
(2) preliminary treatment: with embodiment 9, carry out in hydrolyzer, finishing agent is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.1wt%, and temperature is 100 ℃, and liquor ratio is 1: 10, in 50 minutes processing times, discharges treatment fluid after the preliminary treatment, and washes material;
(3) prehydrolysis: with embodiment 6, carry out in hydrolyzer, hydrolyst is a hydrochloric acid, and process conditions are: concentration of hydrochloric acid is 0.8wt%, and 125 ℃ of temperature, liquor ratio are 1: 10, and hydrolysis time 120 minutes adopts Steam Heating, collects hydrolyzate after the hydrolysis, and washes material;
(4) soda pulping process: with embodiment 3.
Table 1 embodiment hydrolyzate and bamboo dissolved pulp index
(continuous table 1)
(continuous table 1)
(continuous table 1)
Claims (10)
1, a kind of improved prehydrolysis alkaline process is made the method for bamboo dissolved pulp, it is characterized in that: comprise the steps:
(1) bamboo wood is got the raw materials ready, and bamboo wood is made bamboo chip or bamboo silk, and impurity and dust are removed in washing;
(2) preliminary treatment is removed more organic and inorganic impurity, and is made the loss of former relatively bamboo total amount pentosan be less than 2%;
(3) prehydrolysis is carried out in hydrolysis tower or hydrolyzer, and hydrolyst is sulfuric acid or hydrochloric acid, process conditions are: acid concentration is 0.1～10.0wt%, and temperature is 80～140 ℃, and liquor ratio is 1: 4～15, pressure is the saturated vapour pressure under the relevant temperature, and the time is 30～400 minutes;
(4) soda pulping process.
2, improved prehydrolysis alkaline process according to claim 1 is made the method for bamboo dissolved pulp, it is characterized in that: described bamboo wood is cizu, bambusa textile, west wind bamboo, fishscale bamboo, shank bamboo, presss from both sides one or more mixture in bamboo, green bamboo and the square bamboo in vain.
3, improved prehydrolysis alkaline process according to claim 1 and 2 is made the method for bamboo dissolved pulp, it is characterized in that: step 1 comprises chips bamboo wood and/or tears into bamboo chip or bamboo silk, wherein, bamboo chip is of a size of long 15～30mm, wide 10～20mm, thick 3～8mm, and bamboo chip is carried out dither screen, use the water under high pressure spray washing; The bamboo silk is of a size of long 5～40mm, and wherein the bamboo silk of long 20～30mm accounts for more than 70%, and the bamboo silk is washed and remove marrow.
4, improved prehydrolysis alkaline process according to claim 1 is made the method for bamboo dissolved pulp, it is characterized in that: the preliminary treatment of step 2 is carried out in hydrolysis tower or hydrolyzer, finishing agent is sulfuric acid or hydrochloric acid, process conditions are: acid concentration is 0～1.0wt%, temperature is 100～130 ℃, liquor ratio is 1: 5～15, and the time is 30～180 minutes.
5, improved prehydrolysis alkaline process according to claim 1 is made the method for bamboo dissolved pulp, it is characterized in that: in the prehydrolysis of step 3, acid concentration is preferably 0.1～4.0wt%, the hydrolysis stripping ratio of pentosan is not less than 60% in the former bamboo, and the wood sugar yield of pentosan hydrolysis in the former bamboo is not less than 60%.
6, improved prehydrolysis alkaline process according to claim 1 is made the method for bamboo dissolved pulp, it is characterized in that: the soda pulping process of step 4 is the dissolving pulp pulping process based on soda process or sulfate process, comprise boiling in regular turn, selected before floating, bleach, float the selected and process of manufacturing paper with pulp in back.
7, adopt the described improved prehydrolysis alkaline process of claim 1～6 to make the prepared product of method of bamboo dissolved pulp, it is characterized in that: for through step 1 to 3 hydrolyzates that obtain, in the hydrolyzate, concentration of reduced sugar is 1.5～6.0wt%, hydrolyzate purity is not less than 60%, and the wood sugar ratio is not less than 58% in the reducing sugar.
8, at the purposes of the described hydrolyzate product of claim 7, it is characterized in that: described hydrolyzate is used for the preparation of wood sugar, xylitol, L-arabinose or ethanol.
9, adopt the described improved prehydrolysis alkaline process of claim 1～6 to make the prepared product of method of bamboo dissolved pulp, it is characterized in that: for through step 1 to 4 bamboo dissolved pulps that obtain, the every index of bamboo dissolved pulp is: dynamic viscosity is 8.28～9.72mPas, alpha cellulose 〉=93.0%, ash≤0.10%, iron part≤20ppm, whiteness 〉=81%, 0.05～3mm
2Little dust≤140mm
2/ Kg oven-dry weight is greater than 3mm
2Big dust≤1.0/Kg oven-dry weight is inhaled base number 〉=500%, resin≤0.70%, pentosan≤3.00%, lignin trace, the quantitative 600～800g/m of fourdrinier wire
2, the quantitative 400～600g/m of cylinder
2, delivery moisture content 8.5～11.5%.
10, at the purposes of the described bamboo dissolved pulp product of claim 9, it is characterized in that: described bamboo dissolved pulp is used for cellulose viscose pulp, cellulose acetate dissolving pulp, nitrocellulose dissolving pulp or cellulose ether dissolving pulp.
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