US1730383A - of berlin - Google Patents
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- Publication number
- US1730383A US1730383A US1730383DA US1730383A US 1730383 A US1730383 A US 1730383A US 1730383D A US1730383D A US 1730383DA US 1730383 A US1730383 A US 1730383A
- Authority
- US
- United States
- Prior art keywords
- liquor
- pulp
- fiber
- sodium
- cooking
- 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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- 238000010411 cooking Methods 0.000 description 36
- 239000000835 fiber Substances 0.000 description 36
- GEHJYWRUCIMESM-UHFFFAOYSA-L Sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 24
- 238000000034 method Methods 0.000 description 24
- 235000010339 sodium tetraborate Nutrition 0.000 description 24
- 239000000463 material Substances 0.000 description 22
- 239000004328 sodium tetraborate Substances 0.000 description 20
- 239000000243 solution Substances 0.000 description 20
- LSNNMFCWUKXFEE-UHFFFAOYSA-N sulfonic acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 20
- 230000029087 digestion Effects 0.000 description 18
- -1 sodium-boron salts Chemical class 0.000 description 18
- 241001062472 Stokellia anisodon Species 0.000 description 16
- 239000002253 acid Substances 0.000 description 16
- RAHZWNYVWXNFOC-UHFFFAOYSA-N sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 16
- 239000002023 wood Substances 0.000 description 16
- KGBXLFKZBHKPEV-UHFFFAOYSA-N Boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 14
- 239000004327 boric acid Substances 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 14
- 239000000126 substance Substances 0.000 description 14
- LSNNMFCWUKXFEE-UHFFFAOYSA-L Sulphite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 12
- 235000010265 sodium sulphite Nutrition 0.000 description 12
- 238000003723 Smelting Methods 0.000 description 10
- 125000004122 cyclic group Chemical group 0.000 description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 10
- 239000000203 mixture Substances 0.000 description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L na2so4 Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000004291 sulphur dioxide Substances 0.000 description 8
- 235000010269 sulphur dioxide Nutrition 0.000 description 8
- 210000001138 Tears Anatomy 0.000 description 6
- 230000003472 neutralizing Effects 0.000 description 6
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M Sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 238000005649 metathesis reaction Methods 0.000 description 4
- 230000001590 oxidative Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 239000001187 sodium carbonate Substances 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 4
- LVGQIQHJMRUCRM-UHFFFAOYSA-L Calcium bisulfite Chemical compound [Ca+2].OS([O-])=O.OS([O-])=O LVGQIQHJMRUCRM-UHFFFAOYSA-L 0.000 description 2
- 235000009414 Elaeocarpus kirtonii Nutrition 0.000 description 2
- 206010022114 Injury Diseases 0.000 description 2
- 208000007256 Nevus Diseases 0.000 description 2
- 241000218657 Picea Species 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 240000005973 Tabebuia pallida Species 0.000 description 2
- 235000013584 Tabebuia pallida Nutrition 0.000 description 2
- 241001421775 Thereus Species 0.000 description 2
- 229920002522 Wood fibre Polymers 0.000 description 2
- HXOLFXRMWWHLMH-UHFFFAOYSA-L [Na+].[Na+].OB(O)O.[O-]C([O-])=O Chemical compound [Na+].[Na+].OB(O)O.[O-]C([O-])=O HXOLFXRMWWHLMH-UHFFFAOYSA-L 0.000 description 2
- 235000010260 calcium hydrogen sulphite Nutrition 0.000 description 2
- 230000005591 charge neutralization Effects 0.000 description 2
- 238000001311 chemical methods and process Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000003301 hydrolyzing Effects 0.000 description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006011 modification reaction Methods 0.000 description 2
- 230000001264 neutralization Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000004537 pulping Methods 0.000 description 2
- 230000001172 regenerating Effects 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 239000002025 wood fiber 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/04—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
- D21C3/06—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites
Definitions
- This invention relates to a cyclic process of liberating fiber from raw cellulosic materials, such as wood, and has for its object the production of a high grade, easily bleachable pulp, suitable for use, for example, in the manufacture of bond, ledger, and writing papers and as a raw material for the production of a refined fiber of high alpha cellu' lose content.
- sulphur dioxide is suitable for reuse in the pulping of other raw cellulosic material.
- the sodium sulphite is the chemical which under the acid conditions prevailing in the liquor... reacts with and dissolves the encrusting material of the wood, thereby liberating its fibers.
- the sodium sulphite is consumed by reaction, more sodium sulphite is generated according to the reac .tion hereinbefore given, so that the borax is progressively converted into sodium sulphite and free boric acid.
- Boric acid being a comparatively weak or lowly ionized acid, does no injury to the pulp, but apparently aids the sulphurous acid in hydrolyzing the encrusting material.
- the spent liquor resulting from digestion is subsequently neutralized, for instance with sodium carbonate, borax or other sodium-boron salts are again produced, and remain as such during the subsequent smelting operation, the resulting smelt consisting of a mixture of sodium-boron salts such as sodium borate sodium carbonate, and so- S0 content is about 5%.
- the borax used as a raw material may be used in crude condition, that is, as found in nature, the liquor preferably being filtered before being used. Chipped wood, e.
- spruce chips of 7 size may be digested in a cooking liquor of the composition described, under practically the same conditions as are ordinarily maintained during acid sulphite digestion.
- a charge of liquor and chips may be introduccd into the usual digesters of the acid type and then gradually heated to a temperaure of about 255 to 285 F., and brought up to a pressure of about 45 to 75 pounds. After digesting under these conditions for about eight to twelve hours, it will be found that a comparatively high yield of a light colored pulp quite similar in appearance to the ordinary sulphite pulp has been produced.
- the pulp is tested, it will be found that it is characterized by a tear resistance higher than that of the ordinary sulphite pulp, this of course being advantageous in the manufacture of high grade papers.
- the pulp is readily bleachable to whiteness and serves well as a raw material for refining to a white fiber of high alpha cellulose content.
- the desirable characteristics, including high s rength and tear resistance, of a raw pulp produced according to the present invention remain associated with such pulp through subsequent chemical refining treatments, so that such pulp offers advantages over the usual sulphite pulp for use as a raw material in the production of a white wood fiber refined to high alpha cellulose content and intended foruse as a new rag fiber substitute in the manufac ture of high grade papers. 7
- the spent liquor resulting from digestion may be neutralized with borax. sodium carbonate, or other suitable alkaline compounds.
- the chemical used for neutralization may be taken from the smelt while the cycle is being practised, suiiicient additional neutralizing chemical being added along with the smelt chemical to make up losses in the cycle.
- the neutralized spent liquor may then be concentrated as by multipleeifect evaporation to a total solids content of, say, about 50%, whereupon the concentrated liquor may then be de livered into a smelting furnace wherein its combustible content may be burned and its inorganic content smelted, preferably in an oxidizing atmosphere.
- the resulting smelt will consist essentially of sodium-boron salts such as sodium borate, sodium carbonate, and sodium sulphate so that when dissolved with the proper amount of water and acidulated with sulphur dioxide, a liquor suitable for cooking fresh chipped wood is produced.
- sodium-boron salts such as sodium borate, sodium carbonate, and sodium sulphate
- the foregoing example gives a cooking liquor of one composition
- the composition of the liquor may be varied.
- the borax I may employ other fiber-liberating chemicals, such as niter cake (NaHSOQ or salt cake (Na SOQ.
- niter cake NaHSOQ
- salt cake Na SOQ.
- I may also add a certain amount of free boric acid to the cooking liquor, so as to increase the amount of free boric acid present during digestion and thus make possible the realization of a higher percent of sodium borate in the smelt produced from the spent liquor of digestion.
- Boric acid being as already stated a comparatively weak acid, does not, if added in reasonable amount, materially affect the yield 01' quality of the resulting pulp.
- A. process which comprises digesting raw cellulosic material under fiber liberating conditions in a sulphurous acid solution containing sodium-boron salt-s.
- a process which comprises digesting raw cellulosic material under pressure and at elevated temperature in a sulphurous acid solution containing bora-X until fiber liberation has been effected.
- a cyclic process which comprises digesting raw cellulosic material under fiber liberating conditions in a sulphurous acid solution containing boraX, separating the resulting fiber from the spent liquor of digestion, and smelting and recovering the inorganic content of the spent liquor for the prepara tion of a fresh cooking liquor.
- a cyclic process which comprises digesting raw cellulosic material under fiber liber ating conditions in a sulphurous acid solution containing boraX, separating the resulting fiber from the spent liquor, neutralizing and concentrating the spent liquor, burning the combustible content and smelting the inorganic content of the concentrated liquor, and recovering the smelt for the preparation of a fresh cooking liquor.
- a cyclic process which comprises digesting raw cellulosic material under fiber liberating conditions in a sulphurous acid solution containing borax, separating the resulting fiber from the spent liquor, neutralizing and concentrating the spent liquor, burning the combustible content and smelting the inorganic content of the concentrated liquor in an oxidizing atmosphere, recovering the smelt in aqueous solution, and acidulating the solution with sulphur dioxide to produce a fresh cooking liquor.
Description
Patented Oct. 8, 1929 UNITED STATES FATE FFEE GEORGE A. RICHTER, OF BERLIN, NEW HAMPSHIRE, ASSIGNOR TO BROWN COMPAHY, OF BERLIN, NEVI HAMPSHIRE, A CORPORATION OF MAINE GYGLIC PROCESS OF FIBER LIBERATION No Drawing. Application filed May 19,
This invention relates to a cyclic process of liberating fiber from raw cellulosic materials, such as wood, and has for its object the production of a high grade, easily bleachable pulp, suitable for use, for example, in the manufacture of bond, ledger, and writing papers and as a raw material for the production of a refined fiber of high alpha cellu' lose content.
There are at present being commercially practised various chemical processes of fiber liberation from raw cel'lulosic materials such as wood, these processes involving the use of cooking liquors of either an acid or alkaline character and the digestion of the Wood in a chipped condition in the liquor under pressure and at elevated temperature until a liberation of the fibers from the encrusting material of the wood has been effected. One of the widely usedprocesses fortheproductionof an easily bleachable pulp used in the manufacture of high grade white papers is the so-called acid sulphite process, the cooking liquor usually being a sulphurous acid solution of calcium bisulphite. When such a cooking liquor is employed, it is the custom to discharge the spent liquor resulting from digestion into nearby waterways, owing to the difficulty of regenerating the spent liquor economically. Not only does this cause a pollution of the waters into which such spent liquors are discharged and the destruction of piscatorial lite therein, but also a loss of the valuable components of the spent liquor.
I have discovered that it is possible to pr0- duce a high grade pulp by employing a cooking liquor comprising a sulphurous acid solution of sodium-boron salts, such as borax, the temperature, pressure and time necessary for liberating the pulp from Wood being substantially similar to the I conditions maintained when producing the usual commercial sulphite pulp. One of the major advantages of the process of the present invention is that it makes possible an economical cyclic process, as the spent liquor resulting from digestion may be concentrated and its organic content then burned and its inorganic content smelted to produce a smelt which when dissolved in aqueous solution and acidified with 1328. Serial No. 279,205.
sulphur dioxide is suitable for reuse in the pulping of other raw cellulosic material.
l Vhen sodium-boron salts, such as borax, are dissolved in a sulphurous acid solution in producing the cooking liquor of the present invention, a metathesis probably takes place to produce sodium sulphite and free boric acid according to the following equations:
zia s ow H3305 ee oaia so 415 120 Doubtless the sodium sulphite is the chemical which under the acid conditions prevailing in the liquor... reacts with and dissolves the encrusting material of the wood, thereby liberating its fibers. As the sodium sulphite is consumed by reaction, more sodium sulphite is generated according to the reac .tion hereinbefore given, so that the borax is progressively converted into sodium sulphite and free boric acid. Boric acid, being a comparatively weak or lowly ionized acid, does no injury to the pulp, but apparently aids the sulphurous acid in hydrolyzing the encrusting material. Furthermore, being comparatively involatile, it does not escape from the liquor when sulphur dioxide is released thereu from during the latter stages of cooking and so remains in the cooking liquor. Consequently, when the spent liquor resulting from digestion is subsequently neutralized, for instance with sodium carbonate, borax or other sodium-boron salts are again produced, and remain as such during the subsequent smelting operation, the resulting smelt consisting of a mixture of sodium-boron salts such as sodium borate sodium carbonate, and so- S0 content is about 5%. The borax used as a raw material may be used in crude condition, that is, as found in nature, the liquor preferably being filtered before being used. Chipped wood, e. g., spruce chips of 7 size, may be digested in a cooking liquor of the composition described, under practically the same conditions as are ordinarily maintained during acid sulphite digestion. To this end, a charge of liquor and chips may be introduccd into the usual digesters of the acid type and then gradually heated to a temperaure of about 255 to 285 F., and brought up to a pressure of about 45 to 75 pounds. After digesting under these conditions for about eight to twelve hours, it will be found that a comparatively high yield of a light colored pulp quite similar in appearance to the ordinary sulphite pulp has been produced. l i hen the pulp is tested, it will be found that it is characterized by a tear resistance higher than that of the ordinary sulphite pulp, this of course being advantageous in the manufacture of high grade papers. The pulp is readily bleachable to whiteness and serves well as a raw material for refining to a white fiber of high alpha cellulose content. The desirable characteristics, including high s rength and tear resistance, of a raw pulp produced according to the present invention remain associated with such pulp through subsequent chemical refining treatments, so that such pulp offers advantages over the usual sulphite pulp for use as a raw material in the production of a white wood fiber refined to high alpha cellulose content and intended foruse as a new rag fiber substitute in the manufac ture of high grade papers. 7
The spent liquor resulting from digestion may be neutralized with borax. sodium carbonate, or other suitable alkaline compounds. The chemical used for neutralization may be taken from the smelt while the cycle is being practised, suiiicient additional neutralizing chemical being added along with the smelt chemical to make up losses in the cycle. The neutralized spent liquor may then be concentrated as by multipleeifect evaporation to a total solids content of, say, about 50%, whereupon the concentrated liquor may then be de livered into a smelting furnace wherein its combustible content may be burned and its inorganic content smelted, preferably in an oxidizing atmosphere. The resulting smelt will consist essentially of sodium-boron salts such as sodium borate, sodium carbonate, and sodium sulphate so that when dissolved with the proper amount of water and acidulated with sulphur dioxide, a liquor suitable for cooking fresh chipped wood is produced.
lVhile the foregoing example gives a cooking liquor of one composition, it is to be un- 'derstood that the composition of the liquor may be varied. For instance, along with the borax I may employ other fiber-liberating chemicals, such as niter cake (NaHSOQ or salt cake (Na SOQ. These chemicals doubtless undergo metathesis in sulphurous acid solution during cooking to yield sodium sulphite and sulphuric acid, which, of course, is a much stronger acid than boric acid. Apparently as a result of the fact that a cooking liquor in which sodium-boron salts are employed is of weaker acidity than a liquor in which only salt cake or niter cake is employed, I am enabled to produce pulps of higher average fiber lengths and accordingly of greater tear resistance. In other words, owing to the weaker acidity or lower hydrogen ion concentrat-ion in such cooking liquors as I employ in carrying out the process of the present invention, it is quite likely that less fiber hydrolysis takes place during cooking, so that a comparatively high yield of excellent pulp is obtained. I may also add a certain amount of free boric acid to the cooking liquor, so as to increase the amount of free boric acid present during digestion and thus make possible the realization of a higher percent of sodium borate in the smelt produced from the spent liquor of digestion. Boric acid, being as already stated a comparatively weak acid, does not, if added in reasonable amount, materially affect the yield 01' quality of the resulting pulp.
Having thus described certain embodiments of this invention, it is evident that various changes and modifications may be made therein without departing from the spirit or scope of invention as described by the appended claims.
lVhat I claim is 1. A. process which comprises digesting raw cellulosic material under fiber liberating conditions in a sulphurous acid solution containing sodium-boron salt-s.
2. A process which comprises digesting raw cellulosic material under pressure and at elevated temperature in a sulphurous acid solution containing bora-X until fiber liberation has been effected.
3. A cyclic process which comprises digesting raw cellulosic material under fiber liberating conditions in a sulphurous acid solution containing boraX, separating the resulting fiber from the spent liquor of digestion, and smelting and recovering the inorganic content of the spent liquor for the prepara tion of a fresh cooking liquor.
4. A cyclic process which comprises digesting raw cellulosic material under fiber liber ating conditions in a sulphurous acid solution containing boraX, separating the resulting fiber from the spent liquor, neutralizing and concentrating the spent liquor, burning the combustible content and smelting the inorganic content of the concentrated liquor, and recovering the smelt for the preparation of a fresh cooking liquor.
5. A cyclic process which comprises digesting raw cellulosic material under fiber liberating conditions in a sulphurous acid solution containing borax, separating the resulting fiber from the spent liquor, neutralizing and concentrating the spent liquor, burning the combustible content and smelting the inorganic content of the concentrated liquor in an oxidizing atmosphere, recovering the smelt in aqueous solution, and acidulating the solution with sulphur dioxide to produce a fresh cooking liquor.
In testimony whereof I have aliixed my signature.
GEORGE A. RICHTER.
Publications (1)
Publication Number | Publication Date |
---|---|
US1730383A true US1730383A (en) | 1929-10-08 |
Family
ID=3418997
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US1730383D Expired - Lifetime US1730383A (en) | of berlin |
Country Status (1)
Country | Link |
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US (1) | US1730383A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4116759A (en) * | 1975-09-02 | 1978-09-26 | Jan Janson | Preparation of liquor for delignification or alkali treatment by autocaustization, and the preparation of pulp with this liquor |
-
0
- US US1730383D patent/US1730383A/en not_active Expired - Lifetime
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4116759A (en) * | 1975-09-02 | 1978-09-26 | Jan Janson | Preparation of liquor for delignification or alkali treatment by autocaustization, and the preparation of pulp with this liquor |
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