CHAPTER VI.

_TREATMENT OF WOOD._

Chemical Processes.--Watt and Burgess's Process.--Sinclair's

Process.--Keegan's Process.--American Wood Pulp

System.--Aussedat's Process.--Acid Treatment of Wood.--Pictet

and Brélaz's Process.--Barre and Blondel's Process.--Poncharac's

Process.--Young and Pettigrew's Process.--Fridet and Matussière's

Process.

The advantages of wood fibre as a paper material have been fully

recognised in the United States and in many Continental countries,

but more especially in Norway, Sweden, and Germany, from whence

large quantities of wood pulp are imported into this country. There

is no doubt that our home manufacturers have recently paid much

attention to this material, and it is highly probable that wood, as

an inexhaustible source of useful fibre, will at no distant date

hold a foremost rank. Indeed, the very numerous processes which

have been patented since the Watt process was first made known,

indicate that from this unlimited source of fibre the requirements

of the paper-maker may be to a large extent satisfied, provided, of

course, that the processes for reducing the various suitable woods

to the condition of pulp can be economically and satisfactorily

effected. The great attention which this material has received at

the hands of the experimentalist and chemist--the terms not being

always synonymous--shows that the field is considered an important

one, as indeed it is, and if successfully explored will, it is to

be hoped, yield commensurate advantages both to inventors and the

trade.

The object of the numerous inventors who have devised processes

for the disintegration of wood fibre--that is, the separation of

cellulose from the intercellular matters in which the fibres are

enveloped--has necessarily been to dissolve out the latter without

injury to the cellulose itself, but it may be said that as yet the

object has not been fully attained by either of the processes which

have been introduced. To remove the cellular matter from the true

fibre or cellulose, without degrading or sacrificing a portion of

the latter, is by no means easy of accomplishment when practised

on an extensive scale, and many processes which present apparent

advantages in one direction are often found to exhibit contrary

results in another. The field, however, is still an open one, and

human ingenuity may yet discover methods of separating wood fibre

from its surrounding tissues in a still more perfect manner than

hitherto.

The various processes for treating wood for the extraction of its

fibre have been classified into: (1) chemical processes; and (2)

mechanical processes. We will give precedence to the former in

describing the various wood pulp processes, since the pulp produced

by the latter, although extensively used, is chiefly employed,

in combination with other pulps, for common kinds of paper. In

reference to this part of our subject Davis says:--"Experience

has dictated certain improvements in some of the details of

those earlier methods, by which so-called 'chemical wood pulp'

is manufactured very largely on the Continent of Europe.... It

is possible to obtain a pulp of good quality, suitable for some

classes of paper, by boiling the chipped wood in caustic soda, but

when it is desired to use the pulp so prepared for papers having a

perfectly white colour it has been demonstrated in practice that

the action of the caustic soda solution at the high temperature

which is required develops results to a certain degree in weakening

and browning the fibres, and during the past five years much labour

has been expended in the endeavour to overcome the objections

named. The outcome of these efforts has been a number of patents,

having for their object to prevent oxidation and subsequent

weakening of the fibres." In several of these patents, to which we

shall refer hereafter, bisulphite of lime is employed as the agent

to prevent oxidation and consequent degradation of the fibres, and

in other processes bisulphite of magnesia has been used for the

same purpose. Davis further remarks: "Although a common principle

runs through all these methods of preparing cellulose from wood,

they differ in detail, as in the construction of the digesters

employed, methods of treating the wood stock before boiling it in

the sulphurous acid solution, and also as regards pressure, blowing

off the sulphurous acid gas, etc., but all these processes present

a striking similarity to the method patented by Tilghmann in 1867."

There can be no doubt that the action of caustic soda, under high

pressures, is highly injurious both to the colour and strength of

the fibres, and any process that will check this destructive action

in a thoroughly practical way will effect an important desideratum.

=I. Chemical Processes=: _Watt and Burgess's Process_.--This

process, which, with some modifications, is extensively worked

in America, consists in boiling wood shavings, or other similar

vegetable matter, in caustic soda ley, and then washing to remove

the alkali; the wood is next treated with chlorine gas, or an

oxygeneous compound of chlorine, in a suitable vessel, and it is

afterwards washed to free it from the hydrochloric acid formed. It

is now treated with a small quantity of caustic soda in solution,

which instantly converts it into pulp, which only requires to

be washed and bleached, and beaten for an hour and a half in

the beating engine, when the pulp is ready for the machine. The

wood-paper process as carried out in America has been described by

Hofmann, from whose work[15] we have abridged the following:--

The wood, mostly poplar, is brought to the works in 5-feet lengths.

The bark having been stripped off by hand, it is cut into ½-inch

slices by a cutter which consists of four steel knives, from 8

to 10 inches wide by 12 to 15 inches long, which are fastened in

a slightly inclined position to a solid cast-iron disc of about

5 to 7 feet diameter, which revolves at a high speed, chopping

the wood--which is fed to the blades through a trough--into thin

slices across the grain. The trough must be large enough to receive

the logs, usually 10 or 12 inches thick, and it is set at such an

angle that the logs may slide down towards the revolving cutters;

this slanting position only assists the movement of the logs,

while a piston, which is propelled by a rack, pushes them steadily

forward until they are entirely cut up. The piston, or _pusher_,

then returns to its original position, fresh wood is put into the

trough, and the operation repeated. In this way many tons of wood

can be chopped up by one of these cutters in a day. The sliced wood

is conveyed by trucks to an elevator by which it is hoisted up two

storeys to a floor from which the boilers are filled. The boilers

are upright cylinders, about 5 feet in diameter and 16 feet high,

with semi-spherical ends, provided inside with straight perforated

diaphragms, between which the chips from one cord of wood are

confined. A solution of caustic soda, at 12° B., is introduced with

the chips, and fires are started in a furnace underneath. At other

works the boilers are heated by steam circulating through a jacket

which covers the bottom and sides of the boiler.

The boiling is continued for about six hours, when the digestion

is complete, and the contents of the boilers are emptied with

violence, under the pressure of at least 65 lbs. of steam, which

had been maintained inside. A large slide valve is attached to

the side of each boiler for this purpose close to the perforated

diaphragm, and connected by a capacious pipe with a sheet-iron

cylinder of about 12 feet diameter and 10 feet high, which receives

the contents--pulp, liquor, and steam. The object of these large

chambers--one of which serves for two boilers--is to break the

force of the discharging mass. The steam passes through a pipe on

the top of each, and from thence through a water reservoir, while

the liquid containing the pulp flows through a side opening and

short pipe into movable boxes, or drainers, mounted on wheels, and

each capable of holding the contents of one boiler; these boxes are

pushed along a tramway up to the collecting chambers, where the

pulp is received. In a building 132 feet long and 75 feet wide, ten

digesting boilers are arranged in one straight line, and parallel

with the boilers runs the main line of rails, side tracks extending

from it to each of the chambers, and a turn-table is supplied at

every junction. By this arrangement the drainer waggons can be

pushed from the side tracks on to the main line, which leads to

the washing-engines in an adjoining room. A system of drainage

is established below the tramways, by which all the liquid which

drains from the waggons is carried away and collected for treatment

by evaporation; these carriers remain on the side tracks until the

pulp is ready for the washing-engine.

When the greater portion of the liquor has drained off, warm

water is sprinkled over the pulp from a hose for the purpose of

extracting all the liquid which is sufficiently concentrated

to repay the cost of evaporation--the most advantageous method

of recovering the soda. The contents of the waggons--from the

same number of boilers--are then placed in two washing-engines,

each capable of holding 1,000 lbs. of pulp. After being

sufficiently worked in these engines the pulp is transferred

to two stuff-chests, and from thence conveyed by pumps to two

wet-machines. The screens (strainers) of the wet-machines retain

all impurities derived from knots, bark, and other sources, and the

pulp, or half-stuff, obtained is perfectly clean and of a light

grey colour. The pulp is bleached with solution of bleaching powder

like rags, then emptied into drainers and allowed to remain therein

with the liquid for twenty-four to forty-eight hours, or long

enough to render the use of vitriol in the bleaching unnecessary.

The portion of the white pulp which is to be worked up into paper

in the adjoining mill is taken from the drainers into boxes

running on tramways in the moist state, but all the pulp which has

to be shipped to a distance is made into rolls on a large cylinder

paper-machine with many dryers. The object being merely to dry the

pulp, a very heavy web can be obtained, since the water leaves this

pulp very freely. The wood pulp thus obtained is perfectly clean,

of a soft, white spongy fibre, and a greater portion of it is mixed

with a small proportion of rag pulp and worked into book and fine

printing papers. Sometimes the wood pulp is used alone or mixed

with white paper shavings for book paper. The fibres are rather

deficient in strength, but as a material for blotting paper they

are said to be unsurpassed, while the wood paper is much liked by

printers.

The wood from poplar, which is generally preferred, furnishes a

very white fibre, and is easily digested, but since the fibres are

short it is sometimes found advantageous to mix them with longer

fibres, as those of the spruce or pine, although the latter wood

requires a much more severe treatment in boiling with alkali than

the former. In reference to this process the following remarks

appeared in _The Chemist_,[16] 1855:--"The process occupies only

a few hours; in fact, a piece of wood may be converted into

paper and printed upon within twenty-four hours." An interesting

verification of this was published a few years since in an American

paper, the _Southern Trade Gazette_, of Kentucky, which runs as

follows:--"At a wood-pulp mill at Augusta, Ga., a tree was cut

down in the forest at six o'clock A.M., was made into pulp, and

then into paper, at six o'clock in the evening, and distributed

amongst the people as a newspaper by six o'clock the next morning.

From a tree to a newspaper, being read by thousands, in the brief

round of twenty-four hours!" The wood-paper process referred to has

given rise to many subsequent modifications, some of which we will

briefly describe.

=Sinclair's Process.=--The wood is first cut into pieces about

1 inch broad, ⅛th inch thick, and from 2 to 3 inches long. It is

then placed in a boiler and a solution of caustic soda, in the

proportions of 600 gallons to 10 cwts. of dry wood, is poured over

it. The boiler having been securely closed, the heat is raised

till a pressure of 180 to 200 lbs. on the square inch is obtained,

when the fire is withdrawn and the boiler allowed to cool, after

which the ley is blown off, the top door removed, and the contents

scalded. The discharge door is now opened and the pulp transferred

to a poaching-engine to be washed with pure water, when the resin,

&c., are easily removed and the clean fibres obtained, which, it is

said, are longer and firmer than those obtained by other methods.

=Keegan's Process.=--By this method soft deal or pine is sawn up

into pieces from 6 to 12 inches long and ½ inch thick, it being

preferable that all the pieces should be of an equal size, but the

smaller they are the more rapid, of course, will be the operation.

The pieces of timber are placed in a cylindrical boiler, turning

upon a horizontal axis while the digestion is progressing. In a

second boiler is prepared a solution of caustic soda of about 20°

B. (specific gravity 1·161), which is introduced through a pipe

into the first boiler, this being afterwards hermetically closed,

and the soda is forced into the pores of the wood by means of a

pump. When the wood is not more than half an inch in thickness

a pressure of 50 lbs. on the square inch is sufficient, and the

injection of the caustic soda solution is completed in half an

hour. The superabundant liquor is pumped back into the second

boiler for the next operation. The excess of liquor having been

removed from the wood as stated, steam is introduced between the

double sides of the first boiler, and the temperature of the wood

raised from 150° to 190° C. (334° to 438° F.). The wood is next

washed in the usual way until the liquor runs off perfectly limpid,

and the half-stuff thus produced may be converted into pulp either

before or after bleaching, according to the quality and colour of

the paper to be produced.

=American Wood-Pulp System.=--Another method of carrying out the

wood-pulp process has recently been described by Mr. E. A. Congdon,

Ph.B.,[17] from which we extract the following:--"Poplar, pine,

spruce, and occasionally birch, are used in the manufacture of

chemical fibre. Pine and spruce give a longer and tougher fibre

than poplar and birch, but are somewhat harder to treat, requiring

more soda and bleach. Sticks of poplar, freed from bark, and

cleansed from incrusting matter and dirt, are reduced to chips by a

special machine having a heavy iron revolving disc set with knives,

and are then blown by means of a Sturtevant blower into large

stove chambers after passing over a set of sieves having 1¼-inch

for the coarse and 1⅛-inch mesh for the fine sieves, from whence

they pass to the digesters, which are upright boilers 7 by 27

feet, with a manhole at the top for charging the chips and liquor,

and a blow-valve at the bottom for the exit of the boiled wood. A

steam-pipe enters at the bottom, beneath a perforated diaphragm,

and keeps the liquor in perfect circulation during the boiling of

the wood by means of a steam-ejector of special construction."

_Boiling._--The average charge of wood for each digester is 4·33

cords,[18] giving an average yield of 4,140 lbs. of finished fibre

per digester. A charge of 3,400 gallons of caustic soda solution

of 11° B. is given to each digester charged with chips, and the

manhead is then placed in position and steam turned on. Charging

the digester occupies from thirty to forty-five minutes, and steam

is introduced until the gauge indicates a pressure of 110 lbs.,

which occupies about three hours. This pressure is kept up for

seven hours, when it is reduced by allowing the steam to escape

into a large iron tank which acts as a separating chamber for the

spent liquor it carries, the steam entering in at one end and

passing out at the other through a large pipe, the liquor remaining

in the tank. The steam is allowed to escape until the pressure

is reduced to 45 lbs., when the digester is blown. The blow-cap

being removed, the blow-valve is raised and the contents of the

digester are discharged into a pan of iron covered with a suitable

hood. The contents strike against a dash-plate placed midway in

the pan, which thoroughly separates the fibres of the wood. The

time occupied in the foregoing operations is from eleven to eleven

and a half hours. It takes from nine to ten hours to free the pans

from alkali, when they are removed to washing-tanks with perforated

metal bottoms, where the material receives a final washing before

being bleached.

_Washing._--Each of the three digesters has a pan into which

its contents are discharged, and there are also four iron tanks

used for holding the liquors of various strengths obtained

from the cleansing of the pulp and a fifth tank is kept as the

separating-tank before mentioned. When the digester is blown,

the pulp is levelled down with a shovel, and the liquor from the

separating-tank is allowed to flow into it. The contents of the

next strongest pan are pumped upon it, while at the same time the

strongest store tank flows into this pan. This flowing from the

tank to the pan, pumping from here to the pan just blown, and from

there to the evaporators, is kept up until the liquor is not weaker

than 6° B. hot (130° F.). The second pan is now down to 4° B. hot,

and the process of "pumping back" is commenced. The two weakest

tanks are put upon this pan and pumped out of the bottom of it into

the two tanks in which are kept the strongest liquors. The two weak

tanks have been filled in the process of completing the cleansing

of the third pan (the weakest) on which water was pumped until the

last weak tank stood at only ½° B. This pan, now cleaned, is hosed

and pumped over to the washing tanks. A fresh blow is now made in

this pan, and the same treatment kept up as with the first pan.

The foregoing system is thus illustrated by Mr. Congdon:--

Pan A.--Just blown.

" B.--Partly cleaned.

" C.--Almost cleaned.

Tank 1.--3½° B. hot.

" 2.--2° " "

" 3.--1° " "

" 4.--½° " "

Separating tank, strong.

A is levelled down; contents of separating-tank allowed to flow

upon it; B is pumped on to A; at the same time liquor from the two

strong store tanks is put on it (B), and this continued to be sent

from A to the evaporator until it is now weaker than 4° B. hot; the

process of "pumping back" is then commenced. The two weakest are

allowed in succession to flow on to it, and the liquor purified

from the bottom of B into the two strong tanks, filling No. 1,

the stronger, before No. 2. The weakest are filled in the process

of completing the cleansing of C, on which water is pumped until

the last tank from it tests only ½° B. C is now hosed and pumped

over to the washing tanks. A fresh digester is blown in C, and the

process repeated as with A.

The above system has been modified by having an extra pan into

which the liquor from the last pan blown (after sending to the

evaporators until down to 6° hot, and bringing down to 4° hot, by

the stored liquor) is pumped. When the strength is reduced to 4°

the pumping is stopped. The liquor from this pan is put in the next

pan blown, after the liquor from the separating-tank has been put

upon it, whereby an economy in time is effected.

The pulp, after being partially cleaned in the pans, still

contains an appreciable quantity of soda. It is hosed over to the

washing-tanks and receives a final washing with hot water. When the

pulp is thoroughly free from alkali, and the water flowing from

under the tank is colourless, the contents are hosed down by hot

water into the bleaching-tanks. The superfluous water is removed

by revolving washers, and about 1,000 gallons of a solution of

chloride of lime at 4° B. are then introduced, and the contents

agitated as usual. The bleaching occupies about six or seven hours,

when the pulp is pumped into draining tanks, where it is left to

drain down hard, the spent bleach flowing away. The stock is then

hosed and pumped into a washing-tank, where it acquires the proper

consistency for the machine. From here it is pumped into the stuff

chest, whence it goes over a set of screens and on to the machine,

from which the finished fibre is run off on spindles. The rolls

are made of a convenient size to handle, averaging about 100 lbs.

each. The fibre is dried on the machine by passing over a series

of iron cylinders heated by steam. The finished product is a heavy

white sheet, somewhat resembling blotting paper. The whole of the

foregoing operations are stated to occupy forty-five hours.

=Aussedat's Process.=--By this method the wood is disintegrated

by the action of jets of vapour. In one end of a cylindrical

high-pressure boiler, about 4½ feet in diameter and 10 feet high,

is fixed a false bottom, whereby the wood placed upon it may be

removed from the liquor resulting from steam condensed in the

chamber, the whole being mounted on lateral bearings which serve

for the introduction of the vapour, and the wood is fed through a

manhole at the upper end of the boiler. Taps are fixed at the upper

and lower ends for the liquid and uncondensed vapour. The wood

having been placed in the boiler, the jet is gradually turned on in

such a way that at the end of three or four hours the temperature

becomes about 150° C., the pressure being about five atmospheres,

which point is maintained for an hour. As the slightest contact

between the wood and the condensed water would at once discolour

the former, it is essential that the liquid be removed from time to

time by one of the outlets provided for the purpose.

The treatment above described is said to be suitable for all kinds

of wood, and although it is the usual practice to introduce it in

logs about a yard long, any waste wood, as chips, shavings, etc.,

may be used. It is preferable, though not necessary, to remove the

bark, but all rotten wood may be left, as it becomes removed in the

condensed water. The logs, after the above treatment, by which the

fibre is disintegrated and the sap and all matters of a gummy or

resinous nature are removed, are afterwards cut up by any suitable

means into discs of about an inch, according to the nature of the

fibre required. These are then introduced into a breaker, in which

they become converted into half-stuff, which, after being mixed

with a suitable quantity of water is passed through mills provided

with conical stones, in which it becomes reduced to whole-stuff.

The pulp thus prepared is principally used in the manufacture of

the best kinds of cardboard, but more particularly such as is used

by artists, since its light brownish shade is said to improve the

tone of the colours. Bourdillat says that in the above process

the vapour has a chemical as well as a mechanical action, for in

addition to the vapour traversing the cellular tissues of the wood

and dissolving a considerable portion of the cell-constituents,

acetic acid is liberated by the heat, which assists the vapour in

its action on the internal substance of the wood.

=Acid Treatment of Wood.=--A series of processes have been

introduced from time to time, the object of which is to effect

the disintegration of wood fibre by the action of acids. The

first of these "acid processes" was devised by Tilghmann in

1866, in which he employed a solution of sulphurous acid; the

process does not appear to have been successful, however, and

was subsequently abandoned, the same inventor having found that

certain acid sulphites could be used more advantageously. Other

processes have since been introduced, in which wood is treated in a

direct way by the action of strong oxidising acids, as nitric and

nitro-hydrochloric acids, by which the intercellular matters of the

wood become dissolved and the cellulose left in a fibrous condition.

=Pictet and Brélaz's Process.=--By this process wood is subjected

to the action of a vacuum, and also to that of a supersaturated

solution of sulphurous acid at a temperature not exceeding 212° F.

In carrying out the process a solution of sulphurous acid is used,

consisting of, say from ⅕ to ⅓ lb. avoirdupois of sulphurous acid

to each quart of water, and employed under a pressure of from three

to six atmospheres at 212° F. Under these conditions the cementing

substances of the wood "retain their chemical character without a

trace of decomposition of a nature to show carbonisation, while

the liquor completely permeates the wood and dissolves out all the

cementing constituents that envelop the fibres." In carrying out

the process practically, the wood is first cut into small pieces

as usual and charged into a digester of such strength as will

resist the necessary pressure, the interior of which must be lined

with lead. Water is then admitted into the vessel and afterwards

sulphurous acid, from a suitable receiver in which it is stored

in a liquid form until the proportion of acid has reached that

before named, that is, from 100 to 150 quarts of the acid to 1,000

quarts of water. The volume of the bath will be determined by the

absorbing capacity of the wood, and is preferably so regulated

as not to materially exceed that capacity. In practice it is

preferable to form a partial vacuum in the digester, by which

the pores of the wood are opened, when it will be in a condition

to more readily absorb the solution and thereby accelerate the

process of disintegration. When disintegration is effected, which

generally occurs in from twelve to twenty-four hours, according

to the nature of the wood under treatment, the liquor, which is

usually not quite spent in one operation, is transferred to another

digester, a sufficient quantity of water and acid being added to

complete the charge. In order to remove the liquor absorbed by the

wood, the latter is compressed, the digester being connected with

a gas-receiver, into which the free gas escapes and in which it

is collected for use again in subsequent operations. The bath is

heated and kept at a temperature of from 177° to 194° F. by means

of a coil in the digester supplied with steam from a suitable

generator. The wood, after disintegration, undergoes the usual

treatment to convert it into paper pulp, and may thus be readily

bleached by means of chloride of lime. The unaltered by-products

contained in the bath may be recovered and treated for use in the

arts by well-known methods.

=Barre and Blondel's Process= consists in digesting the wood for

twenty-four hours in 50 per cent. nitric acid, used cold, by which

it is converted into a soft fibrous mass. This is next boiled for

some hours in water and afterwards in a solution of carbonate of

soda; it is then bleached in the usual way.

=Poncharac's Process.=--In this process cold nitro-hydrochloric

acid (aqua regia) is employed for disintegrating wood in the

proportions of 94 parts of the latter to 6 parts of nitric acid,

the mixture being made in earthen vessels capable of holding 175

gallons. The wood is allowed to soak in the acid mixture for six to

twelve hours. 132 lbs. of aqua regia are required for 220 lbs. of

wood. When it is desired to operate with a hot liquid, 6 parts of

hydrochloric acid, 4 parts of nitric acid, and 240 parts of water

are used in granite tubs provided with a double bottom, and it is

heated by steam for twelve hours and then washed and crushed.

=Young and Pettigrew's Process.=--These inventors use either nitric

or nitrous acids, and the acid fumes which are liberated are

condensed and reconverted into nitric acid.

=Fridet and Matussière's Process.=--This process, which was

patented in France in 1865, consists in treating wood with

nitro-hydrochloric acid, for which purpose a mixture of 5 to 40 per

cent. of nitric acid and 60 to 95 per cent. of hydrochloric acid

is used, which destroys all the ligneous or intercellular matter

without attacking the cellulose. After the wood (or straw) has been

steeped in the acid mixture, the superfluity is drawn off, and

the remaining solid portion is ground under vertically revolving

millstones. The brownish-coloured pulp thus obtained is afterwards

washed and bleached in the usual way.

It is quite true that cellulose can be obtained from wood and

other vegetable substances by treatment with nitric acid alone,

or with a mixture of nitric and hydrochloric acids, but it will

be readily seen that the employment of such large quantities of

these acids as would be required to effect the object in view on a

practical scale, would be fraught with incalculable difficulties,

amongst which may be mentioned the insuperable difficulty of

obtaining vessels that would resist the powerful corrosive action

of the acids. Moreover, since nitric acid forms with cellulose an

explosive substance (_xyloidin_) of the gun cotton series, the risk

involved in the drying of the cellulose obtained would be quite

sufficient to forbid the use of processes of this nature.

The Art of Paper-Making A Practical Handbook of the Manufacture of Paper from Rags, Esparto, Straw, and Other Fibrous Materials, Including the Manufacture of Pulp from Wood Fibre · 第 6 / 22 章