CN104631173B - A kind of pulping process of extraordinary pulp - Google Patents

A kind of pulping process of extraordinary pulp Download PDF

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Publication number
CN104631173B
CN104631173B CN201510052897.7A CN201510052897A CN104631173B CN 104631173 B CN104631173 B CN 104631173B CN 201510052897 A CN201510052897 A CN 201510052897A CN 104631173 B CN104631173 B CN 104631173B
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pulp
steaming
extraordinary
pot
pulping process
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CN104631173A (en
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周立春
熊钢
刘�文
郑艳民
金昌寿
赵丽君
陈雪峰
王月江
黄小雷
贾程瑛
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Xian White Hillfoot Paper Industry Co Ltd Of Stone Of Yanbian
Quzhou Branch China National Pulp And Paper Research Institute
China National Pulp and Paper Research Institute
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Xian White Hillfoot Paper Industry Co Ltd Of Stone Of Yanbian
Quzhou Branch China National Pulp And Paper Research Institute
China National Pulp and Paper Research Institute
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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
    • D21C3/00Pulping cellulose-containing materials
    • D21C3/02Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • D21C3/022Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes in presence of S-containing compounds

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Paper (AREA)

Abstract

The invention discloses the pulping process of a kind of extraordinary pulp, belong to Pulp and Paper Engineering technical field.The present invention utilizes soluble base ammonium salt or sodium salt, is configured to sulfite liquor, uses pine good timber or pine leftover pieces, produces extraordinary pulp.Production technology includes: the preparation of (1) cooking liquor: total acid is 3~6%, and combined acid is 0.8~1.5%;(2) selection, washing wood chip;(3) dress pot steaming and decocting: add and press-fit pot, two sections of steaming and decoctings;(4) terminal point determining: judge according to the residual acid of red liquid and color.The pulp degree of polymerization produced is more than 2000, and bleachability is 30~50%, and screened yield is 44~55%.Through bleaching, cellulose ethers can be met, cellulose esters manufacturer produces the requirement of high-viscosity products, fill the domestic gaps.

Description

A kind of pulping process of extraordinary pulp
Technical field
The invention belongs to Pulp and Paper Engineering technical field, be specifically related to the pulping process of a kind of extraordinary pulp.
Background technology
External dissolving pulp enterprise is large-scale synthesis group mostly, and production scale is huge, has production dissolving pulp warp for many years Testing, be typically owned by the fast-growing forest land of oneself, raw material is stablized and low price, and dissolving pulp product quality is highly stable, produces into This is relatively low.Additionally, the stimulation increased substantially by China's dissolving pulp demand, in recent years, these enterprises expand the scale of production one after another.State The demand of interior dissolving pulp rises, and stimulates many to starch factory's operation dissolving pulp project, price peak period, viscose rayon enterprise, system Slurry enterprise uses papermaking wood pulp, is further processed into dissolving pulp, is commonly called as " paper changes slurry ".
Within 2010, the domestic dissolving pulp appearance of enterprise utilization of capacity is not enough, and within 2011, situation is worsened, and the price of dissolving pulp is big Width drops, and domestic dissolving pulp enterprise is generally in lossing state, the even stopping production having, and the stopping that new upper dissolving pulp project has is built If some postponements are gone into operation.The main cause causing this phenomenon is global stagflation, and paper making pulps increasess slowly, and southern The slurrying industry in U.S., Southeast Asia etc., has abundant fast-growing woods advantage, is looked forward to being affected by China's dissolving pulp price height, superfluous Slurrying production capacity is changed the line of production dissolving pulp one after another, and promotes to China energetically.Domestic relevant enterprise is absorbed in difficulty condition, is badly in need of the new product of exploitation Product, extricate oneself from a predicament.
For many years, cotton linter is always the raw material of China's dissolving pulp.In recent years, cotton linter price fluctuation is indefinite, viscose glue row Industry yield increases rapidly, promotes China's viscose glue industry raw material progressively to shift to wood pulp.Additionally, state's fast-growing woods resources such as Brazil are rich Richness, wood pulp dissolving pulp is in liberal supply, cheap, and domestic many chemical fiber pulp factories use wood pulps as raw material.
Wood pulp enterprise of China starts late, and raw material sources are unstable, and wood pulp dissolving pulp relies primarily on import, acetifies, is etherified The wood pulps of level can not produce, and production cost also ratio is the highest.The cellulose ether of such as food stage, use the degree of polymerization 1500~ 1800 dissolving pulps manufacture, and all rely on external import.
At present, dissolving pulp about 60% is sulphite wood pulp.Compare with prehydrolytic sulfate process, sulphite process pulp Reactivity worth is preferable, and pulp yield is higher, and shortcoming is that sulphite process does not adapt to some assortment.Cooking liquor alkali calcio is changed Becoming ammonium, sodio soluble base, can expand seeds subject range, ammonium lignin sulfonate is important fertilizer, sodium lignosulfonate It is important chemical products, and ethers high polymerization degree dissolving pulp can only use sulphite process to produce.Big portion of American-European big factory Dividing and use soluble base, domestic research in this respect is the fewest, it is impossible to produce high viscosity dissolving pulp.
Summary of the invention
It is an object of the invention to provide the pulping process of a kind of extraordinary pulp, with solubility ammonium salt, sodium salt as alkali Sulfite pulping process, the pulp degree of polymerization produced be more than 2000, bleachability is 30~50%, screened yield be 44~ 55%, through bleaching, cellulose ethers can be met, cellulose esters manufacturer produces the requirement of high-viscosity products, fills up domestic Blank.
The purpose of the present invention is achieved through the following technical solutions.
The pulping process of the extraordinary pulp of the present invention, step is as follows:
(1) preparation of cooking liquor: use sulfite pulping process, utilize soluble base sodium base or ammonium salt base, Being added by alkali in plant water, be passed through sulfur dioxide gas, cooking liquor consists of total acid 3~6%, combined acid 0.8~1.5%;
(2) selection, washing wood chip: steaming and decocting raw material selects pine good timber or pine leftover pieces, and washing wood chip removes non- Fiber impurity and bark, make wood chip holding 30~the moisture of 60%, and medicinal liquid is impregnated with acceleration, favourable to steaming and decocting early stage;
(3) dress pot steaming and decocting: add and press-fit pot, dress pot pressure is 0.4~0.8MPa, and liquor ratio is 1:(5~6.8), highest pressure For 0.8MPa, by not parking gas maintenance highest pressure during steaming and decocting, using two sections of steaming and decoctings, one period of heating-up time is 2~4h, one Section temperature retention time is 1~3h, and one section of holding temperature is 103~105 DEG C, and the two-stage nitration heating-up time is 1~3h, and two-stage nitration temperature retention time is 15~25h, two-stage nitration holding temperature is 108~130 DEG C, and for maximum temperature of cooking, total cooking time is 19~35h;
(4) terminal point determining: judging terminal by the combined acid in the residual acid of red liquid, terminal combined acid is 0.15~-0.35%, Owing to final stage of cooking generates acid, may cause combined acid is negative value, also by comparison red liquid color auxiliary judgement terminal, with optimum Group or upper one group of red liquid are compared, and reach the equal colors degree of depth and can put pot.
In step (2), wood chip section specification is length 12~17mm, thickness 2~4mm.
In step (3), chip filling amount is 4~6kg, digester capacity and wood chip moisture determine.
Pulping process of the present invention includes that the pulp after putting pot is also performed to discongest, screen and dry, and screen slot is 0.5mm。
The pulp degree of polymerization that pulping process of the present invention prepares is more than 2000, and bleachability is 30~50%, and screened stock obtains Rate is 44~55%, through bleaching, can meet cellulose ethers, cellulose esters manufacturer produces the requirement of high-viscosity products.
The present invention, compared with existing pulping process, has the advantage that and beneficial effect:
(1) comparing with prehydrolytic sulfate process, the reactivity worth of sulphite process pulp is preferable, becomes pulp yield higher, steams Boil liquid alkali and use ammonium, sodio soluble base, can expand assortment subject range, and ethers high polymerization degree dissolving pulp Sulphite process can only be used to produce, and domestic research in this respect is the fewest;
(2) foreign technology monopolization can be broken, break away from the dependence to import high viscosity wood pulps, fill the domestic gaps, right In producing low viscosity dissolving pulp factory, help they clean transformations, break away from current predicament, it is possible to use wood leftover material slurrying, close Reason utilizes timber resources, cost-effective;
(3) compared with tradition sulphite process and external high mucilage sulphite process, this method uses low total acid height chemical combination The thinking that acid, low temperature simmer, uses two sections of steaming and decoctings, and low total acid can reduce acid degradation, and high combined acid is conducive to protection Cellulose and prevent lignin be condensed, temperature is on fibre damage impact maximum, and compared with removing lignin, low temperature is more beneficial for reducing fine Dimension degraded, simmers for a long time and can protect fiber to greatest extent, and two sections of steaming and decoctings can remove lignin as far as possible and reduce fiber Damage;
(4) the pulp degree of polymerization that pulping process of the present invention prepares is more than 2000, belongs to high viscosity pulp, bleachability Being 30~50%, screened yield is 44~55%, through bleaching, can be used to produce cellulose ethers, cellulose esters;
(5) can prepare side-product from the red liquid of steaming and decocting, ammonium lignin sulfonate is important fertilizer, and sodium lignosulfonate is important Industrial chemicals, be the important source of finance of factory.
Accompanying drawing explanation
Fig. 1 is sulfite cooking flow chart.
Detailed description of the invention
Below in conjunction with testing program, result of study and embodiment, the present invention is described further, but application claims The scope of protection is not limited thereto.
Embodiment 1
Cooking liquor preparation bottle adds 20L service water, weighs 300g ammonium hydrogen carbonate, be dissolved in plant water, rock acceleration Dissolve, be passed through sulfur dioxide gas, control gas flow, suitably rock, accelerate the reaction of alkali uniform dissolution, promote carbon dioxide Effusion, measures total acid and the free acid of cooking liquor, calculates combined acid, until total acid 6%, combined acid 1.5%, stops being passed through two Sulfur oxide;
Steaming and decocting raw material selects steaming and decocting raw material to select pine good timber, and section specification is length 12~17mm, thickness 2~4mm, Widths affect is little, rejects relatively chump and wood flour, with factory's water washing wood chip, removes non-fiber impurity, makes wood chip keep Moisture 60%, accelerates medicinal liquid and is impregnated with, favourable to steaming and decocting early stage;
Chip filling amount is 6kg, adds and press-fits pot, and pressure is 0.4MPa, and liquor ratio is 1:5, and highest pressure is 0.8MPa, steaming and decocting Period maintains highest pressure by not parking gas, uses two sections of steaming and decoctings, and one period of heating-up time is 4h, and one section of temperature retention time is 3h, One section of holding temperature 105 DEG C, the two-stage nitration heating-up time is 3h, and two-stage nitration temperature retention time is 20h, and two-stage nitration holding temperature is 130 DEG C, for High-temperature, total cooking time is 30h;
Judging terminal by the combined acid in the residual acid of red liquid, terminal combined acid is 0.15%, also by comparison red liquid color Auxiliary judgement terminal, compares with optimal set or upper one group of red liquid, reaches the equal colors degree of depth and can put pot.
Embodiment 2
Cooking liquor preparation bottle in add 20L service water, weigh 320g sodium carbonate, be dissolved in plant water, rock add instant Solve, be passed through sulfur dioxide gas, control gas flow, suitably rock, accelerate the reaction of alkali uniform dissolution, promote carbon dioxide ease Go out, measure total acid and the free acid of cooking liquor, calculate combined acid, until total acid 5.9%, combined acid 1.4%, stop being passed through two Sulfur oxide;
Pine leftover pieces selected by steaming and decocting raw material, and section specification is length 12~17mm, and thickness 2~4mm, widths affect is not Greatly, reject relatively chump and wood flour, with factory's water washing wood chip, remove non-fiber impurity, make wood chip keep moisture 59%, add Speed medicinal liquid is impregnated with, favourable to steaming and decocting early stage;
Chip filling amount is 5.9kg, adds and press-fits pot, and pressure is 0.7MPa, and liquor ratio is 1:6, and highest pressure is 0.8MPa, steams Boiling period to pass through not park gas maintenance highest pressure, use two sections of steaming and decoctings, one period of heating-up time is 4h, and one section of temperature retention time is 3h, one section of holding temperature 105 DEG C, the two-stage nitration heating-up time is 3h, and two-stage nitration temperature retention time is 21h, and two-stage nitration holding temperature is 129 DEG C, For maximum temperature, total cooking time is 31h;
Judging terminal by the combined acid in the residual acid of red liquid, terminal combined acid is 0.13%, also by comparison red liquid color Auxiliary judgement terminal, compares with optimal set or upper one group of red liquid, reaches the equal colors degree of depth and can put pot.
Embodiment 3
Cooking liquor preparation bottle adds 20L service water, weighs 280g ammonium hydrogen carbonate, be dissolved in plant water, rock acceleration Dissolve, be passed through sulfur dioxide gas, control gas flow, suitably rock, accelerate the reaction of alkali uniform dissolution, promote titanium dioxide Carbon escapes, and measures total acid and the free acid of cooking liquor, calculates combined acid, until total acid 6%, combined acid 1.4%, stop being passed through Sulfur dioxide;
Pine good timber selected by steaming and decocting raw material, and section specification is length 12~17mm, and thickness 2~4mm, widths affect is not Greatly, reject relatively chump and wood flour, with factory's water washing wood chip, remove non-fiber impurity, make wood chip keep moisture 55%, add Speed medicinal liquid is impregnated with, favourable to steaming and decocting early stage;
Chip filling amount is 5.5kg, adds and press-fits pot, and pressure is 0.5MPa, and liquor ratio is 1:6, and highest pressure is 0.8MPa, steams Boiling period to pass through not park gas maintenance highest pressure, use two sections of steaming and decoctings, one period of heating-up time is 4h, and one section of temperature retention time is 3h, one section of holding temperature 105 DEG C, the two-stage nitration heating-up time is 3h, and two-stage nitration temperature retention time is 19h, and two-stage nitration holding temperature is 130 DEG C, For maximum temperature, total cooking time is 29h;
Judging terminal by the combined acid in the residual acid of red liquid, terminal combined acid is 0.11%, also by comparison red liquid color Auxiliary judgement terminal, compares with optimal set or upper one group of red liquid, reaches the equal colors degree of depth and can put pot.

Claims (5)

1. the pulping process of an extraordinary pulp, it is characterised in that comprise the following steps that
(1) preparation of cooking liquor: use sulfite pulping process, utilize soluble base sodium base or ammonium salt base, by salt Base adds in plant water, is passed through sulfur dioxide gas, and cooking liquor consists of total acid 3~6%, combined acid 0.8~1.5%;
(2) selection, washing wood chip: steaming and decocting raw material selects pine good timber or pine leftover pieces, washing wood chip to remove non-fiber Property impurity and bark, make wood chip keep 30~the moisture of 60%, cooking liquor is impregnated with acceleration, favourable to steaming and decocting early stage;
(3) dress pot steaming and decocting: add and press-fit pot, dress pot pressure is 0.4~0.8MPa, and liquor ratio is 1:(5~6.8), highest pressure is 0.8MPa, by not parking gas maintenance highest pressure during steaming and decocting, uses two sections of steaming and decoctings, and one period of heating-up time is 2~4h, one section Temperature retention time is 1~3h, and one section of holding temperature is 103~105 DEG C, and the two-stage nitration heating-up time is 1~3h, and two-stage nitration temperature retention time is 15 ~25h, two-stage nitration holding temperature is 108~130 DEG C, and for maximum temperature of cooking, total cooking time is 19~35h;
(4) terminal point determining: judging terminal by the combined acid in the residual acid of red liquid, terminal combined acid is 0.15~-0.35%, the most logical Cross comparison red liquid color auxiliary judgement terminal, compare with optimal set or upper one group of red liquid, reach the equal colors degree of depth i.e. Pot can be put.
The pulping process of a kind of extraordinary pulp the most according to claim 1, it is characterised in that in described step (2), wood chip is cut Sheet specification is length 12~17mm, thickness 2~4mm.
The pulping process of a kind of extraordinary pulp the most according to claim 1, it is characterised in that wood chip dress in described step (3) Pot amount is 4~6kg, digester capacity and wood chip moisture determine.
The pulping process of a kind of extraordinary pulp the most according to claim 1, it is characterised in that put the pulp after pot and also to enter Row is discongested, screens and is dried, and screen slot is 0.5mm.
The pulping process of a kind of extraordinary pulp the most according to claim 1, it is characterised in that the pulp polymerization prepared Degree is more than 2000, and bleachability is 30~50%, and screened yield is 44~55%, through bleaching, can meet cellulose ethers, cellulose esters Class manufacturer produces the requirement of high-viscosity products.
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