US3560331A - Pulping of wood with sulfite base digestion liquor containing acetic acid - Google Patents
Pulping of wood with sulfite base digestion liquor containing acetic acid Download PDFInfo
- Publication number
- US3560331A US3560331A US709891A US3560331DA US3560331A US 3560331 A US3560331 A US 3560331A US 709891 A US709891 A US 709891A US 3560331D A US3560331D A US 3560331DA US 3560331 A US3560331 A US 3560331A
- Authority
- US
- United States
- Prior art keywords
- acetic acid
- sulfite
- wood
- pulp
- percent
- 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
Links
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title abstract description 89
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 title abstract description 32
- 239000002023 wood Substances 0.000 title abstract description 18
- 238000004537 pulping Methods 0.000 title description 8
- 238000002419 base digestion Methods 0.000 title description 2
- 230000029087 digestion Effects 0.000 abstract description 29
- 229920001131 Pulp (paper) Polymers 0.000 abstract description 5
- XLYOFNOQVPJJNP-PWCQTSIFSA-N Tritiated water Chemical compound [3H]O[3H] XLYOFNOQVPJJNP-PWCQTSIFSA-N 0.000 abstract 1
- 238000000034 method Methods 0.000 description 17
- 238000010411 cooking Methods 0.000 description 16
- 229920002678 cellulose Polymers 0.000 description 10
- 239000001913 cellulose Substances 0.000 description 10
- 238000004061 bleaching Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 5
- 229920003043 Cellulose fiber Polymers 0.000 description 4
- 235000005018 Pinus echinata Nutrition 0.000 description 4
- 241001236219 Pinus echinata Species 0.000 description 4
- 235000017339 Pinus palustris Nutrition 0.000 description 4
- 229920005610 lignin Polymers 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 235000007173 Abies balsamea Nutrition 0.000 description 3
- 229920002581 Glucomannan Polymers 0.000 description 3
- 229920002488 Hemicellulose Polymers 0.000 description 3
- 241000218685 Tsuga Species 0.000 description 3
- 229920002301 cellulose acetate Polymers 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 description 2
- 229920000875 Dissolving pulp Polymers 0.000 description 2
- 229920000057 Mannan Polymers 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 229940046240 glucomannan Drugs 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 240000003021 Tsuga heterophylla Species 0.000 description 1
- 235000008554 Tsuga heterophylla Nutrition 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
- D21C3/003—Pulping cellulose-containing materials with organic compounds
Definitions
- the well-known and widely used sulfite pulping process for the production of refined cellulose fiber suitable for high-grade paper stock and suitable for dissolving or for chemical pulp uses involves digesting wood (preferably in the form of chips) in an aqueous sulfite digestion liquor at elevated temperatures and pressures to solubilize and remove lignin and other unwanted materials from the cellulose.
- the substantially lignin-free cellulosic fiber that results is then removed from the digestion liquor and subjected to various stages of purification (i.e., bleaching) and washing to remove remaining small amounts of lignin and other impurities and then dried.
- Very white, active pulps of substantially pure cellulose fiber are produced in this manner.
- K No. bleachability of an unbleached pulp is customarily measured by means of the well-known standard TAPPI potassium permanganate number (K No.). Other factors being equal, decreasing K Nos. indicate an increasing ease of bleaching.
- Degradation or depolymerization of the cellulose in the pulp is usually measured by determination of the intrinsic viscosity (I.V.) of its solution in a standardized cuene solution. A decreasing I.V. is indicative of increased degradation or depolymerization of the cellulose and as a rule K No. can only be lowered at the expense of reduction of the I.V.
- I.V. intrinsic viscosity
- Glucomannans are one type of hemicellulose that invariably carries over from the wood to appear at least in trace quantities in most dissolving woodpulps.
- I carried out certain experiments in which various amounts of acetic acid replaced some of the water in the sulfite digestion liquors used.
- the addition of the acetic acid lower the glucomannan content of the resultant pulp, but most unexpectedly, when the acetic acid content of the liquor was within certain limits the K No. of the pulp was significantly decreased without any compensating decrease in the I.V.
- sulfite pulping practice involves digesting or cooking wood (usually in the form of chips) in an aqueous sulfite digestion liquor at temperatures ranging from about to C., and pressures of from about 50 to 150 p.s.i.g. for from about 3.5 to 9.0 hours.
- a pulp is produced comprising essentially pure cellulose and a spent liquor containing lignin, soluble carbohydrates, inorganic salts and other soluble or solubilized constituents of the wood.
- the liberated cellulose fiber is then separated from the spent sulfite liquor and purified by various combinations of bleaching, extraction, and washing, and finally dried.
- the result is a reactive, very white, relatively pure cellulose fiber suitable for conversion into high-grade papers and for use in the production of regenerated cellulose and cellulose derivatives such as rayons, cellulose acetates, nitrates, etc.
- the improved process of my invention and the product obtained thereby are based upon my discovery that when about 20 to 75 percent (by volume) of the water in the soluble-base sulfite digestion liquor is replaced by an equal amount of acetic acid, the digestion results in an easy bleaching pulp with an exceptionally high I.V., or conversely a pulp with an exceptionally low K No. for a given I.V.
- the replacement of less than about 20 percent of the water content of the digestion liquor with acetic acid will produce some reduction in the K No./I.V. ratio of the unbleached pulp; however, there is a dramatic and most unexpected reduction in said ratio when the acetic acid is increased above 20 percent.
- some reduction of the K No./I.V. ratio is still obtained at acetic acid replacements in excess of 75 percent by volume, but
- the conditions under which the practice of the invention are most advantageously carried out are essentially the same as those employed in conventional sulfite cooking practices. If a finished bleached product is desired having the same I.V. as a conventional pulp, a compensating increase in the severity of the cooking conditions is required which in turn results in a whiter and purer cellulose end product.
- the length of time, temperature and pressure of a cooking procedure required to obtain a pulp of a specified I.V. and/or K No. are variables that must always be taken into consideration in sulfite cooking operations and the determination of the cooking conditions best adapted to produce a product with desired characteristics in the practice of my invention in a matter well within the skill of workers in this art.
- EXAMPLE 1 Five cooks were made on southern pine chips each using 3.2 kilograms of wood on an oven dry basis in 12 liters of soda base sulfite digestion liquor containing the amounts of acetic acid and under the digestion conditions set out in Table I. The characteristics of the unbleached pulps obtained illustrate the striking increase in bleachability and I.V. afforded by the presence of the indicated percentages of acetic acid (glacial) in the digestion liquors.
- EXAMPLE 4 In a second series of cooks using the process and the same chips as in Example 2, a slight variation in the digestion time at a concentration of 50 percent by volume of acetic acid was made to illustrate how the I.V. ad the K No./I.V. ratio of the unbleached pulp could be varied. From the range of results obtained it is clear that considerable control of the characteristics of the product is easily obtained.
Landscapes
- Paper (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US70989168A | 1968-03-04 | 1968-03-04 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3560331A true US3560331A (en) | 1971-02-02 |
Family
ID=24851706
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US709891A Expired - Lifetime US3560331A (en) | 1968-03-04 | 1968-03-04 | Pulping of wood with sulfite base digestion liquor containing acetic acid |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US3560331A (en)) |
| DE (1) | DE1815667A1 (en)) |
| NO (1) | NO120397B (en)) |
| SE (1) | SE338498B (en)) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4094735A (en) * | 1974-09-06 | 1978-06-13 | Kopparfors Ab | Method of pulping with sulfite liquor containing formic acid esters |
| USRE32408E (en) * | 1982-09-29 | 1987-04-28 | Masonite Corporation | Lignosulfonate-phenol-formaldehyde resin binder |
| US20150051385A1 (en) * | 2012-04-26 | 2015-02-19 | Archer Daniels Midland Company | Liquid / Liquid Separation of Lignocellulosic Biomass to Produce Sugar Syrups and Lignin Fractions |
-
1968
- 1968-03-04 US US709891A patent/US3560331A/en not_active Expired - Lifetime
- 1968-10-01 SE SE13262/68A patent/SE338498B/xx unknown
- 1968-10-12 NO NO4062/68A patent/NO120397B/no unknown
- 1968-12-19 DE DE19681815667 patent/DE1815667A1/de active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4094735A (en) * | 1974-09-06 | 1978-06-13 | Kopparfors Ab | Method of pulping with sulfite liquor containing formic acid esters |
| USRE32408E (en) * | 1982-09-29 | 1987-04-28 | Masonite Corporation | Lignosulfonate-phenol-formaldehyde resin binder |
| US20150051385A1 (en) * | 2012-04-26 | 2015-02-19 | Archer Daniels Midland Company | Liquid / Liquid Separation of Lignocellulosic Biomass to Produce Sugar Syrups and Lignin Fractions |
Also Published As
| Publication number | Publication date |
|---|---|
| NO120397B (en)) | 1970-10-12 |
| DE1815667A1 (de) | 1969-10-16 |
| SE338498B (en)) | 1971-09-06 |
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