US2459570A - Method of refining sulfate turpentine - Google Patents
Method of refining sulfate turpentine Download PDFInfo
- Publication number
- US2459570A US2459570A US757679A US75767947A US2459570A US 2459570 A US2459570 A US 2459570A US 757679 A US757679 A US 757679A US 75767947 A US75767947 A US 75767947A US 2459570 A US2459570 A US 2459570A
- Authority
- US
- United States
- Prior art keywords
- turpentine
- liquor
- mill
- refining
- crude
- 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
- 241000779819 Syncarpia glomulifera Species 0.000 title description 32
- 239000001739 pinus spp. Substances 0.000 title description 32
- 229940036248 turpentine Drugs 0.000 title description 32
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 title description 23
- 238000000034 method Methods 0.000 title description 15
- 238000007670 refining Methods 0.000 title description 5
- 229910021653 sulphate ion Inorganic materials 0.000 description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000010411 cooking Methods 0.000 description 9
- 239000002655 kraft paper Substances 0.000 description 7
- 101100348017 Drosophila melanogaster Nazo gene Proteins 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000002023 wood Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 241000272060 Elapidae Species 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical class [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 4
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000123 paper Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000009993 causticizing Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- -1 dimercaptans Chemical class 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 125000001174 sulfone group Chemical group 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 125000005323 thioketone group Chemical group 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F3/00—Obtaining spirits of turpentine
- C09F3/02—Obtaining spirits of turpentine as a by-product in the paper-pulping process
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S585/00—Chemistry of hydrocarbon compounds
- Y10S585/929—Special chemical considerations
- Y10S585/947—Terpene manufacture or recovery
Definitions
- Patentea anilx 1949 assure METHOD 01'' am G SULFATE George H. fieGregondnternational-Falls, Minn.
- This invention relates to the treatment oi crude turpentine and'more particularly to a'process or deodorizing-turpntines whieh are obtained as a by-product in the..-manuiacture ct, cellulose according to the sulfate process, and alsothe; development. of a product oipleasingodor and of high quality.
- j A iurtherob'iect is the provision in a method of the character described.
- the cellulose material to be treated (usually wood chips) ,together with the usual chemicals are'pl'aced in a dig'esterand steam admitted until thepre'ssure in the digester reaches 110-135 pounds with the consequent temperature within the digester from-about 335 to 350 1".
- Heat is suppliedto thecooking vessel or digester by direct supply of steam or by external heat; the cooking liquor is then "circulated through the cooking vessel during the cooking operation.
- heat with indirect steam the cooking liquor is circulated through the digester and an outside heat exchanger; In the direct heat the steam furnishes circulation by'turbulence within the digester. It is ammmon practice.
- Such compounds may include mercaptans, dimercaptans, thio-ethers, sulphoxides. sulphones, sul- (Cl. sz-z) z r phinic acids, sulphonic acids, disulphides. thioaldahydes, thioketones, esters,,amides and other complex sulphur or nonsulphur compounds.
- Bome'or all of these compounds maybe present 5 in the crude sulphate turpentine, imparting to it an exceedingly ,oilensive odor, the removal of which presents the chief problem in producing sulphate wood turpentine 0! a pleasing and marketable odor. It has been found that this problem is efficiently solved by the present process which is a combination 'of chemical and other steps.
- crude sulphate turpentine refined by ll what may be termed a chemical extraction process employing a material such as kratt mill green liquor;
- the krait pulp mill green liquor is substantially immiscible in crude sulphate turpentine but capable of dissolving, combining with or in some manner in removing odor producing bodies contained therein.
- the process oithe present invention includes intimately contacting the crude sulphate turpentine with krait mill green liquor or its equivalent,
- the upper layer is withdrawn and subjected to further treatment as hereinafter more specifically set forth.
- the lower layer is withdrawn and sent to the krai't mill green liquor storage tank and may be used in the knit process without detriment to such as process. 1
- Example L-About ten parts of crude sulphate turpentine is stirred with about five parts of kraft mill green liquor.
- the krait mill green liquor is preferably added in several increments at a temperature of about to about F. for about ten minutes.
- the material is permitted to stand until the two layers separate.
- the lower layer consists of the green liquor and the odor producing bodies and this is withdrawn and maybe returned to the kraft mill green liquor storage.
- the upper layer consisting oi turpentine is treated with bleaching material-in water such as to calcium hypochlorite.
- bleaching material-in water such as to calcium hypochlorite.
- the amount of available assume 3 chlorine required will vary from about a to about 12% of the weight of the turtine. Suitable agitation is desirable for mixing of the turpentine and the calcium hypochlorite then is contacted for sevcral'hours with activated carbon.
- the turpentine obtained may be subjected to distillation. However, for commercial use the distillation step is not required.
- the amount of treating liquor used in refining the crude sulphate turpentine is based primarily on theamount of sulphur compounds contained in the crude sulphate turpentine. As the sulphur compounds, particularly the mercaptans increase in the crude sulphate turpentine, the amount of treating liquor must be increased to obtain satisfactory results.
- the wood chips are heated under pressure inclosed digesters with an alkaline cooking liquor known as white liquor.
- a typical white liquor contains Sodium hydroxide 4.00 cu. it. as NazO Sodium sulfide 2.17 cu. ft. as NazO Sodium carbonate .93 cu. ft. as NazO
- the composition of the white liquor may vary with difierent woods and different cooking schedules etc. This liquor extracts the lignin and other non-cellulose constituents of the wood and is discharged from the digester at the end of the cook as a dark liquor known as black liquor.
- black liquor is concentrated and the black liquor is then burned or smelted in a furnace with the addition of sodium sulfate.
- the organic matter is burned out in the furnace and the inorganic constituents are recovered which are dissolved in water to form a make-up liquor known as "green liquor.”
- the composition of green liquor is as follows:
- the composition of green liquor may vary from mill to mill. This green liquor is used as a base for making up supplies of white liquor for reuse in the digesters by causticizing it with lime.
- An important feature of the invention resides in the use, as an odor extracting medium, of a solution containing the inorganic constituents normally found in the cycle of a krait paper mill, that is one or more of the constituents of green liquor or white liquor.
- a solution containing the inorganic constituents normally found in the cycle of a krait paper mill that is one or more of the constituents of green liquor or white liquor.
- Such solutions can be withdrawn from the kraft mill cycle, and when the extraction is completed, the spent extracting liquor can be returned to the mill cycle.
- a method of obtaining commercially usable turpentine which comprises, separating crude turpentine from vapors removed from a kraft cooking process, withdrawing green liquor from the kraft mill cycle and mixing such withdrawn liquor with the crude sulphate turpentine, permitting the mixture .to stand until separated into two layers, removing the lower layer and retuming it to the kraft mill cycle and withdrawing the top layer as refined sulphate turpentine.
- a method of refining crude sulphate turpentine to obtain commercially usable turpentine which comprises, extracting from said crude sulphate turpentine odor producing compounds with an aqueous solution containing sodium hydroxide, sodium carbonate and sodium sulfide.
- a method of refining sulphate turpentine containing malodorous compounds which comprises, treating said turpentine with an aqueous solution containing green li'quor as prepared in a kraft paper mill.
- a method of refining crude sulphate turpentine containing malodorous compounds which comprises, adding green liquor'at a temperature of about to about F. to the crude sulphate turpentine, permitting the mixture to stand until separated into two layers, removing the upper layer of turpentine, adding calcium hypochlorite containing from about 4% to about 12% of available chlorine based upon the weight of the turpentine; and thereafter contacting the turpen- REFERENCES CITED
- the following references are of record in the file of this patent:
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Paper (AREA)
Description
Patentea anilx 1949 assure METHOD 01'' am G SULFATE George H. fieGregondnternational-Falls, Minn.
assignor toltllnnesota No Drawing.-
and-Ontario Paper Com- Application June 21, 1941,
' Serial No. "7,879
,1 Q g This invention relates to the treatment oi crude turpentine and'more particularly to a'process or deodorizing-turpntines whieh are obtained as a by-product in the..-manuiacture ct, cellulose according to the sulfate process, and alsothe; development. of a product oipleasingodor and of high quality. j A iurtherob'iect is the provision in a method of the character described. of improved steps for eliminating the offensive and obnoxious odor phate pulp, the cellulose material to be treated (usually wood chips) ,together with the usual chemicals are'pl'aced in a dig'esterand steam admitted until thepre'ssure in the digester reaches 110-135 pounds with the consequent temperature within the digester from-about 335 to 350 1". Heat is suppliedto thecooking vessel or digester by direct supply of steam or by external heat; the cooking liquor is then "circulated through the cooking vessel during the cooking operation. In the case of heat with indirect steam the cooking liquor is circulated through the digester and an outside heat exchanger; In the direct heat the steam furnishes circulation by'turbulence within the digester. It is ammmon practice. to relieve steam and other vapors generated in the digester during cooking operation. Thisremoval is. us'-' ually done as the pressure is'heing increased in vapors are led into a separating devicewhere the condensed oil layer is removed and then sent to storage and the water layersent to waste. The oil' layer is known as crude sulphate wood turpentine.
Due to the presence sodium sulphide in the cooking liquor a number at exceedingly .maiodorr ous sulphur compounds be iormed Such compounds may include mercaptans, dimercaptans, thio-ethers, sulphoxides. sulphones, sul- (Cl. sz-z) z r phinic acids, sulphonic acids, disulphides. thioaldahydes, thioketones, esters,,amides and other complex sulphur or nonsulphur compounds. Bome'or all of these compounds maybe present 5 in the crude sulphate turpentine, imparting to it an exceedingly ,oilensive odor, the removal of which presents the chief problem in producing sulphate wood turpentine 0! a pleasing and marketable odor. It has been found that this problem is efficiently solved by the present process which is a combination 'of chemical and other steps.
In accordance with one aspect of the present invention, crude sulphate turpentine refined by ll what may be termed a chemical extraction process employing a material such as kratt mill green liquor; The krait pulp mill green liquor is substantially immiscible in crude sulphate turpentine but capable of dissolving, combining with or in some manner in removing odor producing bodies contained therein.
The process oithe present invention includes intimately contacting the crude sulphate turpentine with krait mill green liquor or its equivalent,
permitting the mixture to separate into an upper layer composed of refined turpentine and a lower layer composed oi substantially said green liquor and the odor producing bodies contained in the crude sulphate turpentine. The upper layer is withdrawn and subjected to further treatment as hereinafter more specifically set forth. The lower layer is withdrawn and sent to the krai't mill green liquor storage tank and may be used in the knit process without detriment to such as process. 1
In order to disclose the nature of the present invention still more clearly, an illustrative example will hereinaiter be described. It should be clearly understood however, that this is done purely for the purpose of illustration and is .not to .beconsidered a limitation upon the spirit of the scope 01' this invention.
Example L-About ten parts of crude sulphate turpentine is stirred with about five parts of kraft mill green liquor. The krait mill green liquor is preferably added in several increments at a temperature of about to about F. for about ten minutes. The material is permitted to stand until the two layers separate. The lower layer consists of the green liquor and the odor producing bodies and this is withdrawn and maybe returned to the kraft mill green liquor storage. The upper layer consisting oi turpentine is treated with bleaching material-in water such as to calcium hypochlorite. The amount of available assume 3 chlorine required will vary from about a to about 12% of the weight of the turtine. Suitable agitation is desirable for mixing of the turpentine and the calcium hypochlorite then is contacted for sevcral'hours with activated carbon. The
activated carbon removes by absorption residual coloring matter in the turpentine. The result of the foregoing treatment is a mild odored turpentine ready for commercial use. i
I If desired, the turpentine obtained may be subjected to distillation. However, for commercial use the distillation step is not required.
The amount of treating liquor used in refining the crude sulphate turpentine is based primarily on theamount of sulphur compounds contained in the crude sulphate turpentine. As the sulphur compounds, particularly the mercaptans increase in the crude sulphate turpentine, the amount of treating liquor must be increased to obtain satisfactory results.
In the krai't or sulphate process of fiber liberation as heretofore described, the wood chips are heated under pressure inclosed digesters with an alkaline cooking liquor known as white liquor.
A typical white liquor contains Sodium hydroxide 4.00 cu. it. as NazO Sodium sulfide 2.17 cu. ft. as NazO Sodium carbonate .93 cu. ft. as NazO The composition of the white liquor may vary with difierent woods and different cooking schedules etc. This liquor extracts the lignin and other non-cellulose constituents of the wood and is discharged from the digester at the end of the cook as a dark liquor known as black liquor. In ordinary sulfate mill practice, the black liquor is concentrated and the black liquor is then burned or smelted in a furnace with the addition of sodium sulfate. The organic matter is burned out in the furnace and the inorganic constituents are recovered which are dissolved in water to form a make-up liquor known as "green liquor." The composition of green liquor is as follows:
Sodium sulfide 2.19 cu. n. as NazO Sodium hydroxide .32 cu. ft. as NazO Sodium carbonate 4.67 cu. it. as NazO The composition of green liquor may vary from mill to mill. This green liquor is used as a base for making up supplies of white liquor for reuse in the digesters by causticizing it with lime.
An important feature of the invention resides in the use, as an odor extracting medium, of a solution containing the inorganic constituents normally found in the cycle of a krait paper mill, that is one or more of the constituents of green liquor or white liquor. Such solutions can be withdrawn from the kraft mill cycle, and when the extraction is completed, the spent extracting liquor can be returned to the mill cycle.
It will be observed by one skilled in the art that the foregoing specification is subject to modiflcationsand such variations as come within the spirit of the invention are intended to be included in the appended claims.
What is claimed is:
1. A method of obtaining commercially usable turpentine which comprises, separating crude turpentine from vapors removed from a kraft cooking process, withdrawing green liquor from the kraft mill cycle and mixing such withdrawn liquor with the crude sulphate turpentine, permitting the mixture .to stand until separated into two layers, removing the lower layer and retuming it to the kraft mill cycle and withdrawing the top layer as refined sulphate turpentine.
2. A method of refining crude sulphate turpentine to obtain commercially usable turpentine which comprises, extracting from said crude sulphate turpentine odor producing compounds with an aqueous solution containing sodium hydroxide, sodium carbonate and sodium sulfide.
, 3. A method of refining sulphate turpentine containing malodorous compounds which comprises, treating said turpentine with an aqueous solution containing green li'quor as prepared in a kraft paper mill.
4. A method of refining crude sulphate turpentine containing malodorous compounds which comprises, adding green liquor'at a temperature of about to about F. to the crude sulphate turpentine, permitting the mixture to stand until separated into two layers, removing the upper layer of turpentine, adding calcium hypochlorite containing from about 4% to about 12% of available chlorine based upon the weight of the turpentine; and thereafter contacting the turpen- REFERENCES CITED The following references are of record in the file of this patent:
UNITED STATES PATENTS Number Name Date 1,493,454 Jobson May 6, 1924 1,938,693 Gillespie et a]. Dec. 12, 1933 2,283,067 Jennings May 12, 1942 FOREIGN PATENTS Number Country Date Great Britain 1910
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US757679A US2459570A (en) | 1947-06-27 | 1947-06-27 | Method of refining sulfate turpentine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US757679A US2459570A (en) | 1947-06-27 | 1947-06-27 | Method of refining sulfate turpentine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2459570A true US2459570A (en) | 1949-01-18 |
Family
ID=25048779
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US757679A Expired - Lifetime US2459570A (en) | 1947-06-27 | 1947-06-27 | Method of refining sulfate turpentine |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2459570A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2974081A (en) * | 1955-05-19 | 1961-03-07 | Sonoco Products Co | Method for integrating sodium based sulfite and sulfate pulping processes |
| US3158533A (en) * | 1962-09-21 | 1964-11-24 | Improved Machinery Inc | Continuous pulping extraction apparatus |
| US3432402A (en) * | 1967-01-19 | 1969-03-11 | Arizona Chem | Recovery of turpentine from black liquor |
| US4461648A (en) * | 1980-07-11 | 1984-07-24 | Patrick Foody | Method for increasing the accessibility of cellulose in lignocellulosic materials, particularly hardwoods agricultural residues and the like |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB191023467A (en) * | 1910-05-12 | 1911-10-05 | Richter & Richter | A Process for Purifying Hydrocarbons. |
| US1493454A (en) * | 1920-11-22 | 1924-05-06 | New York And Pennsylvania Comp | Process of refining crude turpentine |
| US1938693A (en) * | 1933-06-27 | 1933-12-12 | Bogalusa Paper Company Inc | Process for refining sulphate wood turpentine |
| US2283067A (en) * | 1939-11-02 | 1942-05-12 | William H Jennings | Process for refining sulphate wood turpentine |
-
1947
- 1947-06-27 US US757679A patent/US2459570A/en not_active Expired - Lifetime
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB191023467A (en) * | 1910-05-12 | 1911-10-05 | Richter & Richter | A Process for Purifying Hydrocarbons. |
| US1493454A (en) * | 1920-11-22 | 1924-05-06 | New York And Pennsylvania Comp | Process of refining crude turpentine |
| US1938693A (en) * | 1933-06-27 | 1933-12-12 | Bogalusa Paper Company Inc | Process for refining sulphate wood turpentine |
| US2283067A (en) * | 1939-11-02 | 1942-05-12 | William H Jennings | Process for refining sulphate wood turpentine |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2974081A (en) * | 1955-05-19 | 1961-03-07 | Sonoco Products Co | Method for integrating sodium based sulfite and sulfate pulping processes |
| US3158533A (en) * | 1962-09-21 | 1964-11-24 | Improved Machinery Inc | Continuous pulping extraction apparatus |
| US3432402A (en) * | 1967-01-19 | 1969-03-11 | Arizona Chem | Recovery of turpentine from black liquor |
| US4461648A (en) * | 1980-07-11 | 1984-07-24 | Patrick Foody | Method for increasing the accessibility of cellulose in lignocellulosic materials, particularly hardwoods agricultural residues and the like |
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