US2017985A - Mancfacttjbe of cellulose - Google Patents
Mancfacttjbe of cellulose Download PDFInfo
- Publication number
- US2017985A US2017985A US2017985DA US2017985A US 2017985 A US2017985 A US 2017985A US 2017985D A US2017985D A US 2017985DA US 2017985 A US2017985 A US 2017985A
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- US
- United States
- Prior art keywords
- pulp
- chlorine
- cellulose
- alkali
- per cent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 229920002678 cellulose Polymers 0.000 title description 84
- 239000001913 cellulose Substances 0.000 title description 82
- 239000003513 alkali Substances 0.000 description 92
- 239000000460 chlorine Substances 0.000 description 90
- 229910052801 chlorine Inorganic materials 0.000 description 90
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 90
- 235000010980 cellulose Nutrition 0.000 description 80
- 238000005406 washing Methods 0.000 description 56
- 238000005660 chlorination reaction Methods 0.000 description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 52
- 238000000034 method Methods 0.000 description 46
- 230000029087 digestion Effects 0.000 description 32
- 238000004519 manufacturing process Methods 0.000 description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 30
- 238000004061 bleaching Methods 0.000 description 24
- 239000007788 liquid Substances 0.000 description 20
- 238000006243 chemical reaction Methods 0.000 description 16
- 239000002253 acid Substances 0.000 description 14
- 239000003518 caustics Substances 0.000 description 14
- 239000000126 substance Substances 0.000 description 12
- 239000000835 fiber Substances 0.000 description 10
- 235000011121 sodium hydroxide Nutrition 0.000 description 10
- WQYVRQLZKVEZGA-UHFFFAOYSA-N Hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000005755 formation reaction Methods 0.000 description 6
- 239000002655 kraft paper Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000123 paper Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 229920002955 Art silk Polymers 0.000 description 2
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 229920002301 Cellulose acetate Polymers 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L Magnesium hydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- MFSIEROJJKUHBQ-UHFFFAOYSA-N O.[Cl] Chemical compound O.[Cl] MFSIEROJJKUHBQ-UHFFFAOYSA-N 0.000 description 2
- VRDIULHPQTYCLN-UHFFFAOYSA-N Prothionamide Chemical compound CCCC1=CC(C(N)=S)=CC=N1 VRDIULHPQTYCLN-UHFFFAOYSA-N 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N Sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 2
- 239000005708 Sodium hypochlorite Substances 0.000 description 2
- XIUROWKZWPIAIB-UHFFFAOYSA-N Sulfotep Chemical compound CCOP(=S)(OCC)OP(=S)(OCC)OCC XIUROWKZWPIAIB-UHFFFAOYSA-N 0.000 description 2
- 229940035295 Ting Drugs 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- 238000001311 chemical methods and process Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000002844 continuous Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxyl anion Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 230000001264 neutralization Effects 0.000 description 2
- 230000003472 neutralizing Effects 0.000 description 2
- 235000019645 odor Nutrition 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000002035 prolonged Effects 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-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
- D21C9/08—Removal of fats, resins, pitch or waxes; Chemical or physical purification, i.e. refining, of crude cellulose by removing non-cellulosic contaminants, optionally combined with bleaching
- D21C9/083—Removal of fats, resins, pitch or waxes; Chemical or physical purification, i.e. refining, of crude cellulose by removing non-cellulosic contaminants, optionally combined with bleaching with inorganic compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-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
- D21C9/10—Bleaching ; Apparatus therefor
- D21C9/1026—Other features in bleaching processes
- D21C9/1052—Controlling the process
Definitions
- Our present invention relates to the manufacture of cellulose and, more particularly, contemplates an improvement in, the manufacture of cellulose byalkaline digestion.
- hard sulfite pulps o1 sulfate pulps more particularly so-called kraft pulps,'are preferably subjected to a preliminary treatment with chlorine whereupon the chlorination products are removed by treatment with a weakly alkaline solution in order to promote their degree of digestion and thereby render them more accessible to the subsequent bleaching operation.
- the time of chlorination may be considerably reduced without damaging the fibers by taking care "that in the same proportion as the chlorine .is brought into reaction, the chlorination products "formed are 1 dissolved by the addition of an exactly dosed amount of alkali such that the pH-value of the bath is maintained between .6 and 9, preferably between 7.5 and-8.5.
- hypochlorite the amount of alkali present was so large that hypochlorite was formed. Therefore, the condi- 25 tions of reaction of these known processes were completely different from those of a chlorination according to this invention and, as experiments have proven, by the known processes, the cellulose pulp suifered a strong reduction of 'viscosity and the resistance was greatly injured.
- the formation of hypochlorite is avoided by controlling the addition of the alkali, so to dis-' solve the added quantity is just suificient that the chlorinated 'lignous substances which are soluble in an alkaline solution. When proceeding in this way, the amount of chlorine which may be brought into reaction in a shorter period time,.is greater than that used for an ordinary chlorination in an acid medium.
- the new process also involves the advantage that it completely avoids foaming caused by the formation of carbonic acid which is abimdantly produced particularly in the treatment of kraft pulps rich in ligneous substances.
- the new process can be carried out in any receptacle which guarantees a thorough and rapid mixture of the pulp with the chemical agents, the density of the pulp depending on the capacity of the mixing tank.
- By avoiding the formation of larger quantities of free chlorine in the bath it also becomes possible to work in open vessels, without inconvenience by odors.
- by keeping the reaction of the bath in a more or less neutral state any wear of the armatures, washing drums, and so on is avoided. I
- A. further improvement of the process according to this invention maybe obtained by performing the chlorination in at least two steps with the intercalation of a wash with a solution of alkali whereby the chlorine brought into reaction in the first step may amount to 60 to per cent. of the quantity of chlorine required. Since in the first chlorination, according to our observations, the cellulose is not injured, this 'step may, if required, be carried out in the usual manner. It is only in the second step that the chlorination must be conducted according to the new process, 1. e. simultaneously neutralizing the bath. This is clearly demonstrated by the following two comparative experiments.
- This mode of operation also involves a considerable reduction of the cost for alkali.
- the second step can be carried out with continuous washing with water.
- 1000 kilos of kraft pulp having a Sieber number of 60 are chlorinated with 3.7 per cent. of chlorine in the form of chlorine-water in a hollander provided with a washing drum. To avoid any excess of chlorine in the bath, the chlorination lasts about 2 hours. Then the pulp is thickened, washed, and mixed with such an amount of alkali that the bath contains about'0. 05 per cent. of NaOH. After the alkali has reacted half an hour, the content of the hollander is thoroughly washed. This treatment is followed by a second chlorination with 1.1 per cent. of chlorine while simultaneously adding alkali. The chlorine water is run in, for instance, at a substantial distance before the bucket or the propeller of the holiander near the bottom.
- the alkali required which may be any soluble alkali, used alone or in mixture, however preferably caustic soda, is added in a highly dilute condition at a substantial distance .behind the mixing device where the chlorine is ractically consumed. During the whole chlorination process the bath must be maintained at a pH-value of 6.5 to 9.0. The quantity of NaOH necessary for this efi'ect amounts to about 1.3 per cent., calculated on the quantity of the pulp. This chlorination step likewise lasts about 2 hours, and its duration depends on the intensity of the mixing device or the speed of propulsion of the hollander. When the chlorination is complete the fiber pulp is mixed with so much alkali that its content of NaOH amounts to 0.05 per cent. and after half and hour's reaction the'pulp is thoroughly washed. The cellulose thus obtained has a viscosity of 740 which is practically its original viscosity but the Sieber number has been reduced to about 8.
- the bleaching is conducted preferably at a temperature above 40 0., for instance, between 40 C. and 80 C.
- a process of manufacturing cellulose which comprises treating a cellulose pulp obtained by alkaline digestion with chlorine while'maintain- 5 ing during the chlorination a pH-value between 6 and 9. by continuous addition of alkali.
- a process of manufacturing cellulose which comprises treating a cellulose pulp obtained by alkaline digestion with chlorine while maintain- 50 ing during the chlorination a pH-value between 6 and 9 by continuous addition or alkali, removing part of the treating liquid, and adding a quantity of water equal to the quantity of treating liquid removed.
- a process of manufacturing cellulose- which comprises treating in a first step a cellulose pulp obtained by alkaline digestion with 60 to 80 per cent.' of the chlorine to be employed in the chlorlnating treatment, washing the pulp free from Q acid, treating the pulp in a second step with.
- a process of manufacturing cellulose which I '5 comprises treating in a first step'a cellulose pulp obtained by alkaline digestion with 60 to 80 per cent. of the chlorine to be employed in the chlorinating treatment, washing the pulp free from acid, treating the, pulp in a second step with the 79 further 20 to 40 per cent. of chlorine while maintaining a pH-value between 6 and 9 by continuous addition of alkali, adding to the pulp so much alkali thatits concentration amounts to at least 0.05 per cent., and washing the pulp with water.
- a process of manufacturing cellulose which comprises treating a cellulose pulp obtained by alkaline digestion with chlorine while maintaining during the chlorination a pH-value between 6 and 9 by continuous addition of alkali, removing part of the treating liquid, and adding a quantity 5 of water equal to the quantity of treating liquid removed, adding to the pulp so much alkali that its concentration amounts to at least 0.05 per cent and washing the pulp with water.
- a process of manufacturing cellulose which 10 further 20 to 40 per cent. of chlorine while maintaining a pH-value between 6 and 9 by continuous addition of alkali, adding to the pulp so much alkali that its concentration amounts to at least 0.05 percent, washing the pulp with water, and 2,0; bleaching the pulp while maintaining the .pulp slightlyv alkaline.
- a process of manufacturing cellulose which comprises treating in a. first step a cellulose pulp obtained by alkaline digestion with 60 255 to 80 per cent. of the chlorine to be employed in the chlorinating treatment, washing the pulp free fromacid, treating the pulp in a second step with the further 20 to 40 per cent. of chlorine while maintaining a. pH-value between 6 and 9 by continuous addition of alkali, adding to the pulp so much alkali that its concentration amounts to at least 0.05 per cent., washing the pulp with water, and bleaching the pulp at a temperature of to 80 C. while maintaining $5 the pulp slightly alkaline.
- a process of manufacturing cellulose which comprises treating in a first step a cellulose pulp obtained by alkaline digestion with 60 to 80 per cent. 01 the chlorine to be employed in the chlo- 40 rinating treatment, washing the pulp free from acid, treating the pulp in a second step with the further 20 to 40 per cent. of chlorine while maintaining a pH-value between 6 and 9 by continuous addition of alkali, adding to the pulp so much alkali that its concentration-amounts to at least 0.05 per cent., washing the pulp with water, treating the pulp with a solution of caustic alkali of 5 to 12 per cent. strength, and washing the pulp with water.
- Aprocess of manufacturing cellulose which comprises treating in a first'step a cellulose pulp obtained by alkaline digestion with 60 to 80 per cent of the chlorine to be employed in the chlorinating treatment, washing the pulp free from $5 acid, treating the pulp in a second step with thefurther 20 to 40 per cent. of chlorine while maim taining a pH-value between 6 and 9 by continu ous addition of alkali, adding to the pulp so much alkali that its concentrationamounts to at least 60 0.05 per cent., washing the pulp with water, treating the pulp with a solution of caustic alkali of 5 to 12 per cent. strength, washing the pulp with water, and bleaching the pulp while maintaining the pulp slightly alkaline.
- a process ofmanufacturing cellulose which comprises treating in a first step a cellulose pulp obtained by alkaline digestion with to per cent. of the chlorine to be employed in the chlorinating treatment, washing the pulp free from 7 acid, treating the pulp in a second step with the further 20 to 40 per cent. of chlorine while maintaining a pH-value between 6 and 9 by continuous addition of alkali, adding to the pulp so much alkali that its concentration amounts to at least (5 0.05 per cent, washing the pulp with water, treating the pulp with a solution of caustic alkali of 5 to 12 per cent. strength, washing the pulp with water, and bleaching the pulp at a temperature of 40 to 80 C. while maintaining the pulp slightly alkaline.
- a process of manufacturing cellulose which comprises treating a cellulose pulp obtained-by alkaline digestion with chlorine while maintain-' ing during the chlorination a pH-value between 6 and 9 by continuous addition of alkali, removing part of the treating liquid, and adding a quantity of water equal to the quantity of treating liquid removed, adding to the pulp so much alkali that its concentration amounts to at least 0.05 per cent., washing the pulp with water, treating the pulp with a solution of caustic alkali of 5 to 12 per cent. strength, and washing the pulp with water.
- a process of manufacturing cellulose which comprises treating a cellulose pulp obtained by alkaline digestion with chlorine while maintaining during the chlorination a pH-va-lue between 6 and 9 by continuous addition of alkali, removing part of the treating liquid, and adding a quantity of water equal to the quantity of treating liquid removed, adding to the pulp so much alkali that its concentration amounts to at least 0.05 per cent, washing the pulp with water, treating the pulp with a solution of caustic alkali of 5 to 12 per cent. strength, washing the pulp with water,
- a process of manufacturing cellulose which comprises treating a cellulose pulp obtained by alkaline digestion with chlorine while maintaining during the chlorination a pH-value between 6 and 9 by continuous addition alkali, removing part of the treating liquid, and adding a quantity of water equal to the quantity oiv treating liquid removed, adding to the pulp so much alkali that its concentration amounts to at least 0.05 per cent., washing the pulp with water, treating the pulp with a solution of caustic alkali of to 12 per cent. strength, washing the pulp with water, and bleaching the pulp at a temperature of 40 to 80 C. while maintaining the pulp slightly alkaline.
Description
5 One of its objects is a process of obtaining an Patented Oct. 22, 1935,
UNITED STATES PATENT OFFICE .Aktiengesellsehaft, Frankfort onthe Main, Germany, a corporation of Germany No Drawing. Application Jnne'9, I933, Serial No.
675,116. In Germany June 15, 1932 U '14 Claims.
Our present invention relates to the manufacture of cellulose and, more particularly, contemplates an improvement in, the manufacture of cellulose byalkaline digestion.
improved cellulose by conducting the chlorinating treatment .which follows the alkaline diges- In the same proportion as the chlorination protion in a manner as will be" described hereafter. Another object is the. improved cellulose obtainable by our new process. Further objects will be seen from the detailed specification following I hereafter.
It is known that hard sulfite pulps o1 sulfate pulps, more particularly so-called kraft pulps,'are preferably subjected to a preliminary treatment with chlorine whereupon the chlorination products are removed by treatment with a weakly alkaline solution in order to promote their degree of digestion and thereby render them more accessible to the subsequent bleaching operation.
Careful studies have proven that the pulps, more particularly sulfate pulps, digested in an alkaline medium, suffer a reduction of their viscosity already when subjected to the aforesaid clilorina'ting treatment andytherefore, a loss of solidity. The reason for this'behavior of the pulp lies in'the fact that the reaction between the chlorine which is necessary in rather large quantities for the chlorination of such strongly incrusted pulps and the ligneous matter occurs but comparatively slowly, so. that, when conducting the chlorination under normal conditions, the
' ceeds to the inner layers the chlorination of the water-insoluble incrusts which have already been attacked by the chlorine, becomes more 'difflcult. The chlorine is more and more prevented from reacting with the inner incrusted layers, so that the bath gradually is enriched with chlorine. The consequence of this is a reduction of the viscosity and tensile strength of the cellulose. 'I'hisdrawbackmay be overcome by causing the ligth which becomes acid in the treatment will ntain an excessive amount of free chlorine for chlorine to react at such a 'slow' rate that it is continuously andcompletely absorbed by the incrusts of the cellulose pulp, so-that the incrusts are practically chlorinated in a bath which is free from chlorine. But because in this case the chlorine,'especially during the addition of the last third of the required amount,is consumed only very slowly, the duration of the chlorination would have to be prolonged too long from the commercial point of view.
According to this invention the time of chlorination may be considerably reduced without damaging the fibers by taking care "that in the same proportion as the chlorine .is brought into reaction, the chlorination products "formed are 1 dissolved by the addition of an exactly dosed amount of alkali such that the pH-value of the bath is maintained between .6 and 9, preferably between 7.5 and-8.5. c
It has already been proposed to react oncellulose pulp first with alkali and then with chlorine. gasor to react on cellulose pulps with alkali'and' chlorine simultaneously. In both cases", however.
the amount of alkali present was so large that hypochlorite was formed. Therefore, the condi- 25 tions of reaction of these known processes were completely different from those of a chlorination according to this invention and, as experiments have proven, by the known processes, the cellulose pulp suifered a strong reduction of 'viscosity and the resistance was greatly injured. In contradistinction thereto, according to this invention, the formation of hypochlorite is avoided by controlling the addition of the alkali, so to dis-' solve the added quantity is just suificient that the chlorinated 'lignous substances which are soluble in an alkaline solution. When proceeding in this way, the amount of chlorine which may be brought into reaction in a shorter period time,.is greater than that used for an ordinary chlorination in an acid medium. f
This fact can be explained from what has been set forth above- By maintaining'a' pH-valu'eof about 8 the chlorinated ligneous substances which are soluble in alkali are dissolved oil and the following layers are now readily accessible to the action of the chlorine. The digestion, therc-v 1 fore, takes place in a more umroma more in? tense, and a more rapid manner. In consequence, the bath will not becomeenriched with. chlorine, and the cellulose is not attached. By these means not only an improvement of the 'Sieber number is obtained while the viscosity remains unchanged, butthe treatment conductedunder such mild conditions yields a cellulose of an increased resistance also against chemical influences in'the finishing of the pulp. The new process also involves the advantage that it completely avoids foaming caused by the formation of carbonic acid which is abimdantly produced particularly in the treatment of kraft pulps rich in ligneous substances. The new process can be carried out in any receptacle which guarantees a thorough and rapid mixture of the pulp with the chemical agents, the density of the pulp depending on the capacity of the mixing tank. By avoiding the formation of larger quantities of free chlorine in the bath, it also becomes possible to work in open vessels, without inconvenience by odors. Moreover, by keeping the reaction of the bath in a more or less neutral state, any wear of the armatures, washing drums, and so on is avoided. I
The experiments set forth in the following table have been carried out in such a manner that the bath, after finishing the chlorination step, was alkaline so as to correspond with an 0.05 per cent. caustic soda solution. After this treatment the pulp was washed. The advantages presented by the process according to this invention may be seen from the following table:
as may be efiected, for instance, by lowering the" washing drum into the hollander, because the products already chlorinated absorb a further amount of chlorine besides the amount of chlorine necessary for the'r dissolution in alkali. This observation has b en verified by an experiment carried out while simultaneously washing with water under which conditions with the application of only 4 per cent. of chlorine, a cellulose was produced having a copper viscosity of 791 and a Sieber numberof 13.
Because with sulfate pulp only asmall part of the chlorination products are soluble in water, the continuous washing with water, as-has likewise been established by experiments, when carried out according to the method hitherto in practice, that is without a continuous addition of alkali, could not lead to an improvement.
A. further improvement of the process according to this invention maybe obtained by performing the chlorination in at least two steps with the intercalation of a wash with a solution of alkali whereby the chlorine brought into reaction in the first step may amount to 60 to per cent. of the quantity of chlorine required. Since in the first chlorination, according to our observations, the cellulose is not injured, this 'step may, if required, be carried out in the usual manner. It is only in the second step that the chlorination must be conducted according to the new process, 1. e. simultaneously neutralizing the bath. This is clearly demonstrated by the following two comparative experiments.
This mode of operation also involves a considerable reduction of the cost for alkali.
As a matter of fact the second step can be carried out with continuous washing with water.
The following example illustrates the invention:
1000 kilos of kraft pulp having a Sieber number of 60 are chlorinated with 3.7 per cent. of chlorine in the form of chlorine-water in a hollander provided with a washing drum. To avoid any excess of chlorine in the bath, the chlorination lasts about 2 hours. Then the pulp is thickened, washed, and mixed with such an amount of alkali that the bath contains about'0. 05 per cent. of NaOH. After the alkali has reacted half an hour, the content of the hollander is thoroughly washed. This treatment is followed by a second chlorination with 1.1 per cent. of chlorine while simultaneously adding alkali. The chlorine water is run in, for instance, at a substantial distance before the bucket or the propeller of the holiander near the bottom. The alkali required, which may be any soluble alkali, used alone or in mixture, however preferably caustic soda, is added in a highly dilute condition at a substantial distance .behind the mixing device where the chlorine is ractically consumed. During the whole chlorination process the bath must be maintained at a pH-value of 6.5 to 9.0. The quantity of NaOH necessary for this efi'ect amounts to about 1.3 per cent., calculated on the quantity of the pulp. This chlorination step likewise lasts about 2 hours, and its duration depends on the intensity of the mixing device or the speed of propulsion of the hollander. When the chlorination is complete the fiber pulp is mixed with so much alkali that its content of NaOH amounts to 0.05 per cent. and after half and hour's reaction the'pulp is thoroughly washed. The cellulose thus obtained has a viscosity of 740 which is practically its original viscosity but the Sieber number has been reduced to about 8.
The advantages involved in the method described reside among others in the high quality of the unbleached material, inasmuch as the resistibility of its fibers complies with the highest requirements. At thesame time the pulp has a lower Sieber number than any known, commercial, highly bleachable sulflte pulp or sulfate pulp. Due to its light yellow color, the flexibility of its fibers and their excellent resistibility, its freedom from resin and its low content of incrusts, it is well suited for the preparation of special papers oi any kind.
Due to its low content of ligneous substance such a pulp may be transformed. without strongly impairing its viscosity and the resistibility of the fibers by oxidizing agents such as the chloride of lime or sodium hypochlorite, when employed in the usual concentration, into a product which can' be bleached perfectly white. It is clear that the higher the viscosity of the starting material the more intense may be the bleaching operation for the production of a highly white material. This, also, is one of the special advantages obtained by the new cautious yet vigorous chlorination. The bleaching operation is preferably carried out as it 6 is described in U. S. Patent 1,801,876, 1. e. while maintaining the reaction slightly alkaline in the bleaching operation by the addition of a small quantity of a caustic alkali, a hydroxide of the alkaline earths including magnesium hydroxide. The bleaching is conducted preferably at a temperature above 40 0., for instance, between 40 C. and 80 C.
All the advantages presented bythe present invention come out, however, much more distinctly, if an unbleached sulfatep'ulp, after chlorinating the same in the manner described, to dissolve out its hemi-cellulose and increase its contents of alpha-cellulose, is first subjected to an. alkaline refinement and then to a bleaching operation. 80 Thus there can be obtained 'highly viscous improved celluloses which not only aresuitable for the preparation of special papers, but can also be employed for chemical processes, for instance the manufacture of artificial silk, such as viscose silk I or cellulose acetate silk. The process, furthermore, involves the advantage that such refined cellulose, the viscosity of which has been greatly spared, can be transformed into products of a lower viscosity which are exceptionally white, by.
l. A process of manufacturing cellulose which comprises treating a cellulose pulp obtained by alkaline digestion with chlorine while'maintain- 5 ing during the chlorination a pH-value between 6 and 9. by continuous addition of alkali.
2. A process of manufacturing cellulose which comprises treating a cellulose pulp obtained by alkaline digestion with chlorine while maintain- 50 ing during the chlorination a pH-value between 6 and 9 by continuous addition or alkali, removing part of the treating liquid, and adding a quantity of water equal to the quantity of treating liquid removed. I
55 3. A process of manufacturing cellulose-which comprises treating in a first step a cellulose pulp obtained by alkaline digestion with 60 to 80 per cent.' of the chlorine to be employed in the chlorlnating treatment, washing the pulp free from Q acid, treating the pulp in a second step with. the
further to 40 per cent. of chlorine while maintaining a pH-value between 6 and 9 by continuous addition of alkali.
4. A process of manufacturing cellulose which I '5 comprises treating in a first step'a cellulose pulp obtained by alkaline digestion with 60 to 80 per cent. of the chlorine to be employed in the chlorinating treatment, washing the pulp free from acid, treating the, pulp in a second step with the 79 further 20 to 40 per cent. of chlorine while maintaining a pH-value between 6 and 9 by continuous addition of alkali, adding to the pulp so much alkali thatits concentration amounts to at least 0.05 per cent., and washing the pulp with water.
1 5. A process of manufacturing cellulose which comprises treating a cellulose pulp obtained by alkaline digestion with chlorine while maintaining during the chlorination a pH-value between 6 and 9 by continuous addition of alkali, removing part of the treating liquid, and adding a quantity 5 of water equal to the quantity of treating liquid removed, adding to the pulp so much alkali that its concentration amounts to at least 0.05 per cent and washing the pulp with water.-
6. A process of manufacturing cellulose which 10 further 20 to 40 per cent. of chlorine while maintaining a pH-value between 6 and 9 by continuous addition of alkali, adding to the pulp so much alkali that its concentration amounts to at least 0.05 percent, washing the pulp with water, and 2,0; bleaching the pulp while maintaining the .pulp slightlyv alkaline.
'I. A process of manufacturing cellulose which comprises treating in a. first step a cellulose pulp obtained by alkaline digestion with 60 255 to 80 per cent. of the chlorine to be employed in the chlorinating treatment, washing the pulp free fromacid, treating the pulp in a second step with the further 20 to 40 per cent. of chlorine while maintaining a. pH-value between 6 and 9 by continuous addition of alkali, adding to the pulp so much alkali that its concentration amounts to at least 0.05 per cent., washing the pulp with water, and bleaching the pulp at a temperature of to 80 C. while maintaining $5 the pulp slightly alkaline.
8. A process of manufacturing cellulose which comprises treating in a first step a cellulose pulp obtained by alkaline digestion with 60 to 80 per cent. 01 the chlorine to be employed in the chlo- 40 rinating treatment, washing the pulp free from acid, treating the pulp in a second step with the further 20 to 40 per cent. of chlorine while maintaining a pH-value between 6 and 9 by continuous addition of alkali, adding to the pulp so much alkali that its concentration-amounts to at least 0.05 per cent., washing the pulp with water, treating the pulp with a solution of caustic alkali of 5 to 12 per cent. strength, and washing the pulp with water.
9. Aprocess of manufacturing cellulose which comprises treating in a first'step a cellulose pulp obtained by alkaline digestion with 60 to 80 per cent of the chlorine to be employed in the chlorinating treatment, washing the pulp free from $5 acid, treating the pulp in a second step with thefurther 20 to 40 per cent. of chlorine while maim taining a pH-value between 6 and 9 by continu ous addition of alkali, adding to the pulp so much alkali that its concentrationamounts to at least 60 0.05 per cent., washing the pulp with water, treating the pulp with a solution of caustic alkali of 5 to 12 per cent. strength, washing the pulp with water, and bleaching the pulp while maintaining the pulp slightly alkaline.
10. A process ofmanufacturing cellulose which comprises treating in a first step a cellulose pulp obtained by alkaline digestion with to per cent. of the chlorine to be employed in the chlorinating treatment, washing the pulp free from 7 acid, treating the pulp in a second step with the further 20 to 40 per cent. of chlorine while maintaining a pH-value between 6 and 9 by continuous addition of alkali, adding to the pulp so much alkali that its concentration amounts to at least (5 0.05 per cent, washing the pulp with water, treating the pulp with a solution of caustic alkali of 5 to 12 per cent. strength, washing the pulp with water, and bleaching the pulp at a temperature of 40 to 80 C. while maintaining the pulp slightly alkaline.
11. A process of manufacturing cellulose which comprises treating a cellulose pulp obtained-by alkaline digestion with chlorine while maintain-' ing during the chlorination a pH-value between 6 and 9 by continuous addition of alkali, removing part of the treating liquid, and adding a quantity of water equal to the quantity of treating liquid removed, adding to the pulp so much alkali that its concentration amounts to at least 0.05 per cent., washing the pulp with water, treating the pulp with a solution of caustic alkali of 5 to 12 per cent. strength, and washing the pulp with water. Y
12. A process of manufacturing cellulose which comprises treating a cellulose pulp obtained by alkaline digestion with chlorine while maintaining during the chlorination a pH-va-lue between 6 and 9 by continuous addition of alkali, removing part of the treating liquid, and adding a quantity of water equal to the quantity of treating liquid removed, adding to the pulp so much alkali that its concentration amounts to at least 0.05 per cent, washing the pulp with water, treating the pulp with a solution of caustic alkali of 5 to 12 per cent. strength, washing the pulp with water,
and bleaching the pulp while maintaining the pulp slightly alkaline.
- 13. A process of manufacturing cellulose which comprises treating a cellulose pulp obtained by alkaline digestion with chlorine while maintaining during the chlorination a pH-value between 6 and 9 by continuous addition alkali, removing part of the treating liquid, and adding a quantity of water equal to the quantity oiv treating liquid removed, adding to the pulp so much alkali that its concentration amounts to at least 0.05 per cent., washing the pulp with water, treating the pulp with a solution of caustic alkali of to 12 per cent. strength, washing the pulp with water, and bleaching the pulp at a temperature of 40 to 80 C. while maintaining the pulp slightly alkaline.
14. An unbleached cellulose pulp produced by alkaline digestion and to a great extent freed from impurities, said pulp having a viscosity of about 700 and a Sieber-number of about 10.
' ERICH OPFERMANN.
GUSTAV-ADOLF FELDTMANN.
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US2017985A true US2017985A (en) | 1935-10-22 |
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US2017985D Expired - Lifetime US2017985A (en) | Mancfacttjbe of cellulose |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3062610A (en) * | 1959-02-10 | 1962-11-06 | Kroy Unshrinkable Wools Ltd | Process for shrinkproofing wool |
US3177111A (en) * | 1962-12-06 | 1965-04-06 | Weyerhaeuser Co | Hypochlorite sulfamic acid process of bleaching cellulosic materials |
WO1988009842A1 (en) * | 1987-06-04 | 1988-12-15 | Carnoe Nils Bertil | A method of reducing chlorophenol compounds in the chlorine bleaching of pulp |
-
0
- US US2017985D patent/US2017985A/en not_active Expired - Lifetime
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3062610A (en) * | 1959-02-10 | 1962-11-06 | Kroy Unshrinkable Wools Ltd | Process for shrinkproofing wool |
US3177111A (en) * | 1962-12-06 | 1965-04-06 | Weyerhaeuser Co | Hypochlorite sulfamic acid process of bleaching cellulosic materials |
WO1988009842A1 (en) * | 1987-06-04 | 1988-12-15 | Carnoe Nils Bertil | A method of reducing chlorophenol compounds in the chlorine bleaching of pulp |
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