CN108867130A - The pulping process of high yield pulp1 needlebush dissolving pulp and its dissolving pulp of preparation - Google Patents

The pulping process of high yield pulp1 needlebush dissolving pulp and its dissolving pulp of preparation Download PDF

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CN108867130A
CN108867130A CN201810388227.6A CN201810388227A CN108867130A CN 108867130 A CN108867130 A CN 108867130A CN 201810388227 A CN201810388227 A CN 201810388227A CN 108867130 A CN108867130 A CN 108867130A
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dissolving pulp
bleaching
temperature
liquor
hydrogen peroxide
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刘秋娟
何亮
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Tianjin University of Science and Technology
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Tianjin University of Science and Technology
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C7/00Digesters
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00Pulping cellulose-containing materials
    • D21C3/02Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/10Bleaching ; Apparatus therefor
    • D21C9/12Bleaching ; Apparatus therefor with halogens or halogen-containing compounds
    • D21C9/14Bleaching ; Apparatus therefor with halogens or halogen-containing compounds with ClO2 or chlorites

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Paper (AREA)

Abstract

This application provides a kind of pulping process of high yield pulp1 needlebush dissolving pulp.The pulping process is successively made through cooking liquor pre-preg, kraft cooking, cold alkali density and element chlorine free bleaching step using needle wood raw material, and the temperature of cooking liquor pre-preg is 20~100 DEG C, and the temperature of kraft cooking is 170~185 DEG C.Compared with traditional prehydrolysis sulfate pulp capable of poaching, high-temperature sulfuric acid salt dissolving pulp of the present invention need to only increase cold alkaline extraction section before drift so that hemi-cellulose content is reduced to appropriate level, and the waste liquid of cold alkaline extraction section can be reused for the boiling stage, not cause increased costs.This technique has universality for the slurry factory production dissolving pulp with sulfate pulping production line, it only needs to change boiling intensity, the slurry that different stage can be produced on same production line, realizes that the slurry of output is converted between paper pulp and dissolving pulp, to increase the product diversity of enterprise;So that enterprise is produced the slurry of different purposes according to the variation in market at any time, improves the ability to ward off risks of itself.

Description

The pulping process of high yield pulp1 needlebush dissolving pulp and its dissolving pulp of preparation
Technical field
The present invention relates to pulp and paper industry field more particularly to a kind of pulping process of high yield pulp1 needlebush dissolving pulp.
Background technique
China is textile production big country, and average annual textile fabric yield ranks first in the world.But it is limited by land resource, grain and cotton Strive ground, town and country strive ground contradiction it is outstanding day by day, the natural fibers such as cotton, fiber crops are difficult to meet Development of Textile Industry needs, fiber consumption figure Growth will rely primarily on the growth of chemical fibre to support.And petrochemicals as chemical fibre raw material are increasingly in short supply, price is held Continue high, obstacle is caused from source to the sustainable development of textile industry.In order to fundamentally solve petroleum resources shortage for Chemical fibre and downstream industry bring adverse effect, with the production of the natural plant fibres raw material such as cotton linter, fiber crops, bamboo and timber Renewable cellulose fibre (i.e. dissolving pulp) is valued by people again.Past 5 years due to cotton price go up, as cotton The short rayon fiber demand of main substitute is spent to be substantially increased, the price of external short rayon fiber is even higher by 10% than cotton.I The demand of state's dissolving pulp surges year by year.Therefore domestic some papermaking enterprises are by the advantage of industry common point to dissolving pulp industry Infiltration.
Currently, being mainly the kraft cooking technique with prehydrolysis by the technique of waste dissolving pulp of timber.It should Method is to carry out prehydrolysis to it before wood chip enters traditional kraft cooking process.The main purpose of prehydrolysis is to reduce Hemicellulose level (especially hemi-cellulose content) in raw material, and change its structure, the alpha-cellulose content of slurry is improved, and control Make its degree of polymerization.In order to reach the general indicator that can float dissolving pulp, half material of hydrolysis is after kraft cooking after prehydrolysis, gained The yield of pulp capable of poaching is generally 30%~35%.Because the yield of dissolving pulp made from this method is relatively low, and make that the production cost increases. In addition, a large amount of pre-hydrolyzed solution can be generated after wood chip prehydrolysis.It is much carried out about to pre-hydrolyzed solution although having had now The report of recycling, and have enterprise to the industrial chemicals in prehydrolysis --- furfural extracts, but is not Whole slurry factories all have the ability to extract the by-product in pre-hydrolyzed solution, and are converted into high value added product.Under normal circumstances, many pre- Hydrolyzing sulfate dissolution slurry factory is to be delivered to alkali collection workshop after mixing pre-hydrolyzed solution with alkaline pulping black liquor, is steamed The operations such as hair, burning, to recycle alkali and thermal energy.In addition, in pre-hydrolysis process, because prehydrolysis temperature is higher by (generally 170 DEG C), the carbohydrate of acid soluble lignin and degradation in plant fiber material also occurs that series of chemical, generates tool Sticking product causes hydrolysis device inner wall serious scale.Therefore, it is necessary to develop a kind of new dissolving pulp boiling and drift White technique avoids the problem that the waste liquid generated by processing prehydrolysis stage and removal reactor dirt layer bring increased costs.
Summary of the invention
On overcoming using soda pulping process delignification and the dynamic (dynamical) feature of carbohydrate degradation The shortcomings that stating the prior art and deficiency provide slurrying and method for bleaching that a kind of needlebush prepares dissolving pulp, close for producing The high yield pulp1 needlebush dissolving pulp of lattice.
To achieve the goals above, according to the one aspect of the application, a kind of high yield pulp1 needlebush dissolving pulp is provided Pulping process.
The pulping process is using needle wood raw material successively through cooking liquor pre-preg, kraft cooking, cold alkali density and nothing Elemental chlorine blanching step is made, and wherein the temperature of cooking liquor pre-preg is 20~100 DEG C, the temperature in kraft cooking step It is 170~185 DEG C.
It further, further include material preparation step before cooking liquor pre-soak step, the material preparation step includes by needle Then the wooden log is whittled into the wood chip of long 15~30mm, 3~5mm of thickness except section, peeling.
Further, in cooking liquor pre-soak step, the alkali charge of cooking liquor is 30%~40% (in terms of NaOH), sulphur Change degree 20%~35%;Liquor ratio is 1:3~1:7, neopelex dosage 0.02%~0.08%, the pre-preg time is 0~150min;
Further, it is directly warming up to 170~185 DEG C after pre-preg process, and is kept the temperature at 170~185 DEG C, into Row kraft cooking, the control heating-up time is 20~100min, soaking time is 60~180min, after boiling, blowing, Dissolving pulp can be floated by being made after cleaning.
Further, element chlorine free bleaching process successively includes:Cold alkali density, the high temperature chlorine dioxide of hydrogen peroxide reinforcing The hot alkali extraction and ClO 2 bleaching section that bleaching, hydrogen peroxide are strengthened.
Further, the cold alkali density process of hydrogen peroxide reinforcing is:It can float after dissolving pulp is broken up and be mixed with the first bleaching liquor It closes, is added in reaction vessel, stirs evenly, 0.5~4h is reacted at 0~50 DEG C, first bleaching liquor is sodium hydroxide, mistake The mixed solution of hydrogen oxide and water, alkali dense are 30~100g/L, and hydrogen peroxide use is 0~2.0%.
Further, high temperature ClO 2 bleaching process is:Resulting slurry after the cold alkali density that hydrogen peroxide is strengthened It cleans, breaks up, be added in reaction vessel after being mixed with the second bleaching liquor, control temperature at 80~100 DEG C, react 0.5~4h, institute State the second bleaching liquor be chlorine dioxide and water mixed solution, Chlorine be 1.0%~3.0%, after drift pH be 1.0~ 5.0。
Further, the hot alkali extraction process of hydrogen peroxide reinforcing is:The resulting slurry of high temperature ClO 2 bleaching is beaten It mixes, is added in reaction vessel with third bleaching liquor after dissipating, 1~3h is reacted at 60~90 DEG C, the third bleaching liquor is hydrogen-oxygen Change the mixed solution of sodium, hydrogen peroxide and water, alkali charge is 1%~5%, and hydrogen peroxide use is 0~2.0%.
Further, ClO 2 bleaching process is:Resulting slurry after the hot alkali extraction of hydrogen peroxide reinforcing is cleaned, It breaks up, is added in reaction vessel after being mixed with the 4th bleaching liquor, is placed in 60~70 DEG C of water bath with thermostatic control, react 1~4h, it is described 4th bleaching liquor be chlorine dioxide and water mixed solution, Chlorine be 0.5%~2.0%, after drift pH be 2.0~ 5.0。
To achieve the goals above, according to further aspect of the application, slurrying disclosed by the invention is additionally provided The dissolving pulp product that method is prepared.
The characteristics of dissolving pulp, is as follows:The hemi-cellulose content of dissolving pulp be 3.0% hereinafter, whiteness be not less than 89%, first kind Content of cellulose is greater than 94.5%, and ash content is not higher than 0.07%.
Pulping process provided by the invention and its dissolving pulp being prepared have the beneficial effect that:
The problem of sample does not need prehydrolysis, easy to operate, no pre-hydrolyzed solution disposition and pre-hydrolysis device fouling, and boiling Pulp yield is higher (being about higher by 6%) afterwards, and poly-pentose is also slightly higher (being about higher by 2%).With traditional prehydrolysis sulfate pulp capable of poaching phase Than high-temperature sulfuric acid salt dissolving pulp of the present invention need to only increase cold alkaline extraction section before drift so that hemi-cellulose content is reduced to Appropriate level, and the waste liquid of cold alkaline extraction section can be reused for the boiling stage, not cause increased costs.Because being not necessarily to prehydrolysis Device, technique described in this method have universality for the slurry factory production dissolving pulp generally with sulfate production line.Only need Change boiling intensity, so that it may which the slurry that different stage is produced on same production line realizes the pulp of output in paper pulp and molten It is converted between solution slurry, to increase the product diversity of enterprise;Enterprise is set to produce difference according to the variation in market at any time The slurry of purposes improves the ability to ward off risks of itself.
Specific embodiment
It is well known that the hemi-cellulose content of needlebush is generally in 8%~12%, with finished product dissolving pulp, hemi-cellulose content is wanted (≤4%) is asked to compare, itself hemi-cellulose content is not just very high.Compared with leaf wood (hemi-cellulose content is about 20%), It does not need to carry out prehydrolysis before kraft cooking, hemi-cellulose content is greatly reduced.After general prehydrolysis, hydrolysis half is expected Hemi-cellulose content in (needlebush and leaf wood) is 8% or so, if further decreasing hemi-cellulose content, yield (30%~ 35%) it will further decrease.It is therefore contemplated that when the wooden dissolving pulp of needle, unlike leaf wood, it is necessary to carry out prehydrolysis Carry out boiling again afterwards;But the feature for combining the hemi-cellulose content of needlebush lower, it makes full use of in sulfate cooking process, The kinetics feature of lignin, cellulose, hemicellulose, a kind of technique for being suitable for the wooden dissolving pulp of needle of optimization.
During soda pulping process, the side-chain radical 4-O- methyl glucose uronic acid of xylan in hemicellulose, in high temperature Under the action of highly basic, generate hexenuronic acid (HexA).And under alkaline environment, HexA ratio 4-O- methyl glucose uronic acid it is steady It is qualitative much higher, so 4-O- methyl glucose uronic acid group transformations are HexA under conditions of temperature is more than 120 DEG C, from And it protects poly-pentose and degrades less.Therefore, the formation of HexA is very unfavorable to dissolving pulp requirement abjection poly-pentose, The generation of this reaction should be avoided or reduced as far as possible.According to soda pulping process carbohydrate kinetics it is found that poly- (140 DEG C of >) could be dissolved out under the higher temperature of pentose.Therefore, it can use the formation of HexA (120 DEG C or so initially form) The characteristics of a large amount of hydrolysis (140 DEG C of hydrolysis temperature >) occur with poly-pentose as far as possible the shortening heating-up time, is directly entered most Carbohydrate and a large amount of basic hydrolysis of lignin are carried out under high-temperature, to reduce the production quantity of HexA, increase poly-pentose Dissolution rate;Meanwhile the degree of polymerization is slurried in removing lignin, adjustment at high temperature.However, will certainly be made if directly shortening the heating-up time The problem of at half steaming.Therefore, the present invention proposes before entering heating, carries out lye pre-preg to wood chip.Specific slurrying Method mainly includes boiling and method for bleaching, and main flow is the cold alkali density-nothing of low temperature prepregs stain-high-temperature sulfuric acid bisulfite cooking- Element chlorine bleaching, specifically in order carry out the step of be:
1) then needlebush log is whittled into long 15~30mm, 3~5mm of thickness wood chip except section, peeling.After wood chip screening, Moisture is measured, in case subsequent boiling is used;
2) medical fluid (sodium hydroxide+vulcanized sodium+neopelex+water) is prepared as desired, with step 1) Gained wood chip mixes, and carries out low temperature prepregs stain;
3) low temperature prepregs stain:Wood chip and cooking liquor are fitted into boiling vessel, presoaked at being 20~100 DEG C in temperature Stain, alkali charge are 30%~40% (in terms of NaOH), sulphidity 20%~35%;Liquor ratio 1:3~1:7, dodecyl benzene sulfonic acid Sodium dosage 0.02%~0.08%, 0~150min of pre-preg;
4) thermophilic digestion:It is directly warming up to maximum temperature of cooking after step 3) the pre-preg process, and most Kept the temperature under high boiling temperature, maximum temperature is 170~185 DEG C, the heating-up time is 20~100min, soaking time be 60~ 180min.After boiling, blowing.The Softwood salt method that can be made into the high yield pulp1 after cleaning can float dissolution Slurry.
5) the cold alkali density (CCE that hydrogen peroxide is strengthenedP):After slurry obtained by step 4) is broken up and medical fluid (sodium hydroxide+ Hydrogen peroxide+water) mixing, be added in reaction vessel, stir evenly, at 0~50 DEG C react 0.5~4h, alkali dense be 30~ 100g/L or so, H2O2Dosage is 0~2.0%;
6) high temperature ClO 2 bleaching section (D0):Slurry obtained by step 5) is cleaned, is broken up, with medical fluid (chlorine dioxide+ Water) mixing after be added in reaction vessel, control temperature at 80~100 DEG C, react 0.5~4h, ClO2Dosage be 1.0%~ 3.0%, pH is 1.0~5.0 after drift;
7) hot alkali extraction (HCE that hydrogen peroxide is strengthenedP):After slurry obtained by step 6) is broken up and medical fluid (sodium hydroxide+ Hydrogen peroxide+water) mixing, it is added in reaction vessel, 1~3h is reacted at 60~90 DEG C, alkali charge is 1%~5% left The right side, H2O2Dosage is 0~2.0%;
8) ClO 2 bleaching section (D1):Slurry obtained by step 7) is cleaned, is broken up, it is mixed with medical fluid (chlorine dioxide+water) It is added in reaction vessel, is placed in 60~70 DEG C of water bath with thermostatic control after conjunction, react 1~4h, ClO2Dosage be 0.5%~ 2.0%, pH is 2.0~5.0 after drift.Finally slurry, which is cleaned, can be obtained up-to-standard dissolving pulp.
It is right below in conjunction with the embodiment of the present application in order to make those skilled in the art more fully understand application scheme Technical solution in the embodiment of the present application is clearly and completely described, it is clear that described embodiment is only the application one Partial embodiment, instead of all the embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not having Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present application.
It should be noted that the term term " includes " of the description and claims of this application and his any change Shape, it is intended that cover it is non-exclusive include, for example, containing the method for series of steps or process is not necessarily limited to clearly arrange Those of out step, but may include other steps being not clearly listed or intrinsic for these methods or process.It is right For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific conditions.
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase Mutually combination.
Embodiment 1
For the present embodiment using pine as research object, the pulping process of the high yield pulp1 needlebush dissolving pulp provided includes by suitable The following steps that sequence carries out:
Kraft cooking step:
1) pine log is whittled into the wood chip of long 15~30mm, 3~5mm of thickness, air-dries and balances after mixing except section after peeling Moisture, in case subsequent boiling is used;
2) it is mixed after preparing cooking liquor with wood chip;Wherein, cooking liquor is sodium hydroxide, vulcanized sodium, detergent alkylate The mixed solution of sodium sulfonate and water.
3) low temperature prepregs stain:Wood chip and cooking liquor are fitted into boiling vessel, pre-preg is carried out at being 25 DEG C in temperature, uses alkali Amount is 36% (NaOH meter), sulphidity 25%, liquor ratio 1:5, neopelex dosage 0.05%, pre-preg 90min, with Half material is made;
4) thermophilic digestion:It is directly warming up to maximum temperature after pre-preg and keeps the temperature;Heating-up time is 60min, most 180 DEG C of high-temperature, 90min, last blowing are kept the temperature, the masson pine sulfate process that can be made into the high yield pulp1 after cleaning can float Dissolving pulp.
Embodiment 2:
For the present embodiment using pine as research object, the pulping process of the high yield pulp1 pine dissolving pulp provided includes by suitable The following steps that sequence carries out:
Kraft cooking step:
1) pine log is whittled into the wood chip of long 15~30mm, 3~5mm of thickness, air-dries and balances after mixing except section after peeling Moisture, in case subsequent boiling is used;
2) it will be mixed after cooking liquor being prepared with wood chip;Wherein, cooking liquor is sodium hydroxide, vulcanized sodium, dodecyl The mixed solution of benzene sulfonic acid sodium salt and water.
3) low temperature prepregs stain:Wood chip and cooking liquor are fitted into boiling vessel, pre-preg is carried out at being 25 DEG C in temperature, uses alkali Amount is 32% (NaOH meter), sulphidity 25%;Liquor ratio 1:5, neopelex dosage 0.05%, pre-preg 90min, with Half material is made;
4) thermophilic digestion:It is directly warming up to maximum temperature after pre-preg, then keeps the temperature;Heating-up time is 60min, 180 DEG C of maximum temperature, 120min is kept the temperature, last blowing can be made into the masson pine sulfate process of the high yield pulp1 after cleaning Dissolving pulp can be floated.
Embodiment 3:
For the present embodiment using masson pine as research object, the pulping process of the high yield pulp1 needlebush dissolving pulp provided includes by suitable The following steps that sequence carries out:
Kraft cooking step:
1) masson pine log is whittled into the wood chip of long 15~30mm, 3~5mm of thickness, air-dries and balances after mixing except section after peeling Moisture, in case subsequent boiling is used;
2) it is mixed after preparing cooking liquor with wood chip;Wherein, cooking liquor is sodium hydroxide, vulcanized sodium, detergent alkylate The mixed solution of sodium sulfonate and water.
3) low temperature prepregs stain:Wood chip and cooking liquor are fitted into boiling vessel, pre-preg is carried out at being 25 DEG C in temperature, uses alkali Amount is 32% (NaOH meter), sulphidity 25%;Liquor ratio 1:5, neopelex dosage 0.05%, pre-preg 120min, Half slurry is made;
4) thermophilic digestion:It is directly warming up under maximum temperature and keeps the temperature after pre-preg;Heating-up time is 80min, most 180 DEG C of high-temperature, 140min is kept the temperature, last blowing, the masson pine sulfate process that can be made into the high yield pulp1 after cleaning can Float dissolving pulp.
Embodiment 4:
The present embodiment does not float sulfate dissolving pulp as research object using prepared by high-temperature sulfuric acid bisulfite cooking, and what is provided is high The method for bleaching of rate needlebush dissolving pulp includes the following steps carried out in order:
Element chlorine free bleaching step:
1) the cold alkali density (CCE that hydrogen peroxide is strengthenedP):It can will float made from 1 boiling method through the foregoing embodiment molten Solution slurry mixes after breaing up with the first bleaching liquor, is added in reaction vessel, and 1~4h is reacted at 40 DEG C, and the first bleaching liquor is hydrogen-oxygen Change the mixed solution of sodium, hydrogen peroxide and water, alkali dense is 50~100g/L, H2O2Dosage is 0~1%;
2) high temperature ClO 2 bleaching section (D0):By CCEPTreated, and slurry is cleaned, and is broken up, after mixing with the second bleaching liquor It is added in reaction vessel, in 90~100 DEG C of at a temperature of 1~4h of reaction, the second bleaching liquor is molten for the mixing of chlorine dioxide and water Liquid, ClO2Dosage is 1.5%~3.5%, and pH is 1.5~4.5 after drift;
3) hot alkali extraction (HCE that hydrogen peroxide is strengthenedP):By D0Treated mixes with third bleaching liquor after slurry breaks up, and adds Enter into reaction vessel, 1~3h is reacted at 70~90 DEG C, third bleaching liquor is that the mixing of sodium hydroxide, hydrogen peroxide and water is molten Liquid, alkali charge are 1%~5%, H2O2Dosage is 0~1%;
4) ClO 2 bleaching section (D1):By HCEPTreated, and slurry is cleaned, and is broken up, is added after mixing with the 4th bleaching liquor Into reaction vessel, 1~4h is reacted at 70~90 DEG C, the 4th bleaching liquor is the mixed solution of chlorine dioxide and water, ClO2Dosage It is 0.3%~1.2%, pH is 2.0~4.5 after drift, finally cleans slurry up to qualified dissolution slurry.
Experimental example 1:Cooking effect evaluation
In order to verify the effect for radiating pine kraft dissolving pulp pulping process of high yield pulp1 provided by the invention, Shen of the present invention It asks someone to have carried out the dissolving pulp prepared by above-described embodiment 1 into embodiment 3 quality testing, and according to traditional prehydrolysis The dissolving pulp that sulfate process is prepared as a comparison, the results are shown in Table 1:
1 sulphate cook method of table and traditional prehydrolysis sulfate cooking process
Note:Prehydrolysis 1 and 2 is respectively using pine and masson pine wood chip as research object.Prehydrolysis condition is:Liquor ratio 1: 6,170 DEG C of maximum temperature, heating-up time 90min, soaking time 60min.Wherein, prehydrolysis 2 by the way of displacement cooking into Row.Displacement cooking is in such a way that temperature is filled and heat fills two sections plus alkali, heat direct heating and heat preservation after filling, and other conditions are:Temperature Fill a section temperature be 120 DEG C, time 40min;Heat fills 160 DEG C of section temperature, time 30min;170 DEG C of soaking zone temperature, heating and Soaking time 180min.
The data of embodiment 1 to embodiment 3 can be seen that according to this boiling method to pine and masson pine from table 1 When carrying out boiling, it is small (12~14) to be slurried Kappa number fluctuation range, screened yield between 36~41%, the degree of polymerization 550~ Between 700, hemi-cellulose content is between 5.0%~6.3%.With traditional intermittent (prehydrolysis 1) and displaced type (prehydrolysis 2) The pine that prehydrolytic sulfate process is produced is compared with the masson pine prehydrolyzed kraft dregs of rice, and yield is about higher by 4% to 7%. Meanwhile the degree of polymerization of the pulp in prehydrolysis 1 and 2 is higher, if reaching the targeted degree of polymerization (for 500) of viscose rayon pulp, Then need to expend more drifts agent (such as H2O2).Compared with the control group, hemi-cellulose content in pulp made from high-temperature sulfuric acid salt method It is slightly higher, it is higher by about 2%.In order to reach the standard of viscose rayon pulp Grade A in national standard, need to carry out cold alkali to it before drift Pre- extracting.
Experimental example 2:Bleaching effect evaluation
Present invention applicant uses (CCEP)-D0-(HCEP)-D1Bleaching method is to this boiling method and conventional boil method system Standby needlebush dissolving pulp out is bleached.
With high-temperature sulfuric acid salt boiling method (alkali pre-preg time 3h, temperature 45 C;Boiling alkali charge 34%, sulphidity 25%, neopelex dosage 0.05%, liquor ratio 1:5.5, heating-up time 1.5h, 180 DEG C of maximum temperature, soaking time 150min) gained masson s pine pulp is bleaching magma;Starching sample property is:Kappa number is 12.1, DP 585, yield 37.42%, Hemi-cellulose content is 6.10%.
With high-temperature sulfuric acid salt boiling method (alkali pre-preg time 3h, temperature 45 C;Boiling alkali charge 32%, sulphidity 25%, neopelex dosage 0.05%, liquor ratio 1:5, heating-up time 1.5h, 180 DEG C of maximum temperature, soaking time 120min) gained pine slurry is bleaching magma.Starching sample property is:Kappa number is 12.2, the degree of polymerization 594, hemi-cellulose content It is 6.07%.
Respectively by both the above brown stock according to following two CCEP~D0~HCEP~D1Process conditions are located respectively Reason:
Pine slurry:Cold alkali density (CCEP):Alkali dense 70g/L, time 2h, slurry dense 10%, 40 DEG C of temperature;D0Section ClO2With 2.5%, bleaching time 1h are measured, 95 DEG C of temperature, slurry dense 10% floats whole pH3.0~3.5;EPSection alkali charge 1%, H2O2Dosage 0.2%, time 1h, 85 DEG C of temperature, slurry dense 10%;D1Section ClO2Dosage 0.3%, time 1h, 85 DEG C of temperature, drift end pH4.5~ 5.0。
Masson s pine pulp:Cold alkali density (CCEP):Alkali dense 70g/L, time 2h, slurry dense 10%, 40 DEG C of temperature;D0Section ClO2With 2.5%, bleaching time 1h are measured, 95 DEG C of temperature, slurry dense 10% floats whole pH3.0~3.5;EPSection alkali charge 1%, H2O2Dosage 0.2%, time 0.5h, 85 DEG C of temperature, slurry dense 10%;D1Section ClO2Dosage 0.3%, time 1h, 85 DEG C of temperature, drift end pH4.5~ 5.0。
Under the above conditions respectively to not floating masson pine and pine dissolving pulp is bleached, and with masson pine prehydrolysis sulphur Hydrochlorate method is compared after can floating dissolving pulp (2 gained of prehydrolysis) bleaching.Prehydrolytic sulfate process can float used in dissolving pulp Bleaching process is E0D0E1D1Four sections of drifts.Specifically bleaching process is:Dense each section of bleached pulp is 10%;E0Section bleaching time 1.5h, 85 DEG C of temperature, NaOH dosage 2%;D0Section bleaching time 1.5h, 95 DEG C of temperature, ClO2Dosage 2%, drift end pH4.0;E1Section Bleaching time 1.5h, 85 DEG C of temperature, NaOH dosage 3%, H2O2Dosage 0.5%; D1Section bleaching time 3h, 85 DEG C of temperature, ClO2 Dosage 0.5%, drift end pH4.0.
Chemical composition, the whiteness of finished product pulp after bleaching are as shown in table 2.By finished product pulp property in table 2 and industry mark About the requirement of Grade A it is found that finished product pulp has reached the standard of viscose rayon needlebush pulp Grade A in standard.And with Prehydrolyzed kraft is compared, and indices do not have much difference.Therefore, in D0EDCold alkali process is carried out before bleaching Poly-pentose (about 2%) content slightly higher in high temperature Softwood salt dissolving pulp is dropped into suitable value, to adapt to viscose rayon Production.
Chemical composition, the whiteness of finished product pulp after table 2 is bleached
Above-described each embodiment, only embodiments of the present invention, when implementation of the present invention cannot be limited with this Range, i.e., all simple equivalence changes carried out according to scope of the present invention patent and patent specification content with repair Decorations, are all still covered by the present invention within the scope of the patent.The foregoing is only a preferred embodiment of the present invention, is not used to limit The system present invention, for those skilled in the art, the invention may be variously modified and varied.It is all in spirit of the invention Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of pulping process of high yield pulp1 needlebush dissolving pulp, which is characterized in that successively pre- through cooking liquor with needle wood raw material Dipping, kraft cooking, cold alkali density and element chlorine free bleaching step are made, and the temperature of cooking liquor pre-preg is 20~100 DEG C, the temperature in kraft cooking step is 170~185 DEG C.
2. the pulping process of high yield pulp1 needlebush dissolving pulp according to claim 1, which is characterized in that presoaked in cooking liquor Further include material preparation step before stain step, the material preparation step include then needlebush log is whittled into except section, peeling it is long by 15~ The wood chip of 30mm, 3~5mm of thickness.
3. the pulping process of high yield pulp1 needlebush dissolving pulp according to claim 1, which is characterized in that presoaked in cooking liquor In stain step, the alkali charge of cooking liquor is 30%~40% (in terms of NaOH), sulphidity 20%~35%;Liquor ratio is 1:3~1: 7, neopelex dosage 0.02%~0.08%, the pre-preg time is 0~150min.
4. the pulping process of high yield pulp1 needlebush dissolving pulp according to claim 3, which is characterized in that pre-preg process knot Directly be warming up to 170~185 DEG C after beam, and kept the temperature at 170~185 DEG C, carry out kraft cooking, control the heating-up time be 20~100min, soaking time are 60~180min, and after boiling, blowing, dissolving pulp can be floated by being made after cleaning.
5. the pulping process of high yield pulp1 needlebush dissolving pulp according to claim 4, which is characterized in that element chlorine free bleaching Process successively includes:Hydrogen peroxide strengthen cold alkali density, high temperature ClO 2 bleaching, hydrogen peroxide strengthen hot alkali extraction and ClO 2 bleaching section.
6. the pulping process of high yield pulp1 needlebush dissolving pulp according to claim 5, which is characterized in that hydrogen peroxide is strengthened Cold alkali density process be:It can float after dissolving pulp is broken up and be mixed with the first bleaching liquor, be added in reaction vessel, stir evenly, 0.5~4h is reacted at 0~50 DEG C, first bleaching liquor is the mixed solution of sodium hydroxide, hydrogen peroxide and water, alkali dense 30 ~100g/L, hydrogen peroxide use are 0~2.0%.
7. the pulping process of high yield pulp1 needlebush dissolving pulp according to claim 5, which is characterized in that high temperature chlorine dioxide Bleaching process is:Resulting slurry after the cold alkali density of hydrogen peroxide reinforcing is cleaned, breaks up, is added after being mixed with the second bleaching liquor Into reaction vessel, temperature is controlled at 80~100 DEG C, reacts 0.5~4h, and second bleaching liquor is the mixing of chlorine dioxide and water Solution, Chlorine are 1.0%~3.0%, and pH is 1.0~5.0 after drift.
8. the pulping process of high yield pulp1 needlebush dissolving pulp according to claim 5, which is characterized in that hydrogen peroxide is strengthened Hot alkali extraction process be:It is mixed after the resulting slurry of high temperature ClO 2 bleaching is broken up with third bleaching liquor, is added to reaction In container, 1~3h is reacted at 60~90 DEG C, the third bleaching liquor is the mixed solution of sodium hydroxide, hydrogen peroxide and water, is used Alkali number is 1%~5%, and hydrogen peroxide use is 0~2.0%.
9. the pulping process of high yield pulp1 needlebush dissolving pulp according to claim 5, which is characterized in that ClO 2 bleaching Process is:Resulting slurry after the hot alkali extraction of hydrogen peroxide reinforcing is cleaned, is broken up, is added to after being mixed with the 4th bleaching liquor anti- It answers in container, is placed in 60~70 DEG C of water bath with thermostatic control, react 1~4h, the 4th bleaching liquor is the mixing of chlorine dioxide and water Solution, Chlorine are 0.5%~2.0%, and pH is 2.0~5.0 after drift.
10. a kind of dissolving pulp being prepared by the described in any item pulping process of claim 1-9, which is characterized in that dissolution The hemi-cellulose content of slurry is 3.0% hereinafter, whiteness is not less than 89%, and content of alphacellulose is greater than 94.5%, and ash content is not higher than 0.07%.
CN201810388227.6A 2018-04-26 2018-04-26 The pulping process of high yield pulp1 needlebush dissolving pulp and its dissolving pulp of preparation Pending CN108867130A (en)

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Publication number Priority date Publication date Assignee Title
CN110644270A (en) * 2019-08-27 2020-01-03 齐鲁工业大学 Process for producing dissolving pulp by TCF bleaching of poplar KP pulp
SE2250793A1 (en) * 2022-06-27 2023-12-28 Valmet Oy Method for processing cellulose pulp obtained from a kraft process
CN117390870A (en) * 2023-10-25 2024-01-12 齐鲁工业大学(山东省科学院) Pulping dynamics model based on reducing sugar and soluble solid content

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CN101484632A (en) * 2006-05-10 2009-07-15 连津格股份公司 Process for producing a pulp
CN102493256A (en) * 2011-12-07 2012-06-13 湖南骏泰浆纸有限责任公司 Eucalyptus dissolving pulp and production method thereof
CN104153229A (en) * 2014-07-16 2014-11-19 华南理工大学 Preparation method of bamboo dissolving pulp
CN104379833A (en) * 2012-05-28 2015-02-25 索德拉细胞公司 New process and a dissolving pulp manufactured by the process

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JP4192565B2 (en) * 2002-11-19 2008-12-10 日本製紙株式会社 Method for producing high whiteness bleached kraft pulp
CN101484632A (en) * 2006-05-10 2009-07-15 连津格股份公司 Process for producing a pulp
CN102493256A (en) * 2011-12-07 2012-06-13 湖南骏泰浆纸有限责任公司 Eucalyptus dissolving pulp and production method thereof
CN104379833A (en) * 2012-05-28 2015-02-25 索德拉细胞公司 New process and a dissolving pulp manufactured by the process
CN104153229A (en) * 2014-07-16 2014-11-19 华南理工大学 Preparation method of bamboo dissolving pulp

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110644270A (en) * 2019-08-27 2020-01-03 齐鲁工业大学 Process for producing dissolving pulp by TCF bleaching of poplar KP pulp
CN110644270B (en) * 2019-08-27 2022-01-07 齐鲁工业大学 Process for producing dissolving pulp by TCF bleaching of poplar KP pulp
SE2250793A1 (en) * 2022-06-27 2023-12-28 Valmet Oy Method for processing cellulose pulp obtained from a kraft process
WO2024005685A1 (en) * 2022-06-27 2024-01-04 Valmet Ab Method for processing cellulose pulp obtained from a kraft process
CN117390870A (en) * 2023-10-25 2024-01-12 齐鲁工业大学(山东省科学院) Pulping dynamics model based on reducing sugar and soluble solid content
CN117390870B (en) * 2023-10-25 2024-03-19 齐鲁工业大学(山东省科学院) Pulping dynamics model based on reducing sugar and soluble solid content

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Application publication date: 20181123