US1863654A - Purification of wood sugar - Google Patents
Purification of wood sugar Download PDFInfo
- Publication number
- US1863654A US1863654A US376502A US37650229A US1863654A US 1863654 A US1863654 A US 1863654A US 376502 A US376502 A US 376502A US 37650229 A US37650229 A US 37650229A US 1863654 A US1863654 A US 1863654A
- Authority
- US
- United States
- Prior art keywords
- sugar
- hydrochloric acid
- wood
- solvent
- alcohol
- 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
- SRBFZHDQGSBBOR-LECHCGJUSA-N alpha-D-xylose Chemical compound O[C@@H]1CO[C@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-LECHCGJUSA-N 0.000 title description 22
- 229960003487 xylose Drugs 0.000 title description 22
- 238000000746 purification Methods 0.000 title 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 52
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 33
- 239000002904 solvent Substances 0.000 description 21
- 239000000203 mixture Substances 0.000 description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- 239000002023 wood Substances 0.000 description 12
- 230000003301 hydrolyzing effect Effects 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000000889 atomisation Methods 0.000 description 9
- 239000012043 crude product Substances 0.000 description 9
- 238000001035 drying Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 229920002678 cellulose Polymers 0.000 description 8
- 239000001913 cellulose Substances 0.000 description 8
- 239000006188 syrup Substances 0.000 description 8
- 235000020357 syrup Nutrition 0.000 description 8
- 238000005245 sintering Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 239000001117 sulphuric acid Substances 0.000 description 3
- 235000011149 sulphuric acid Nutrition 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- -1 chlorine ions Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000011877 solvent mixture Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K1/00—Glucose; Glucose-containing syrups
- C13K1/02—Glucose; Glucose-containing syrups obtained by saccharification of cellulosic materials
Definitions
- Wood sugar which is obtained by the hydrolysis of wood with concentrated hydrochloric acid, may be -freed, to a very large extent, from the excess hydrochloric acid if 5 the wood sugar solution in a finely atomized state is brought into contact with a hotcurrent of air '(see U. S. A. patent specification No. 1,678,819).
- the so-called dry-sugar obtained in this way still'posscsses two undesirable properties; it isa light, voluminous powder-consisting of particles of irregular shapes and large surfaces, which is therefore, ill-suited for transport and further working up, and also it contains resinous impurities 1 and always remnants of hydrochloric acid, which are detrimental for many purposes.
- the hydrochloric acid'present in the dry sugar can be separated by means of certain organic solvents by mere d'ecantation of the same from the sugar and simultaneously the sugar is converted into a syrup of high specific gravity.
- the organic solvents suitable for this purpose are organic liquids containing oxygen which dissolve hydrochloric acid readily and sugar with difficulty. They are soluble in water.
- the separation of sugar and hydrochloric acid may,
- a mixture of 95 %'alcohol with benzene in the ratio of 5: 1 has proved to be particularly suitabld It is then suflicient to 'heat the mixture to 50--6 0. inorder to produce the desired sintering.
- the presence of benzene depresses the solubility of the sugar in alcohol and raises its absorption capability for the resinous extraneous constituents of the dry-sugar, I
- the separation of sugar and solvent and the simultaneous conversion of the sugar'into a syrup form may also be attained by adding a 7 small quantity of water to the mixture of sugar and aIeohoLbenZene.
- Ewamples 9 1. 1000 guns. of dry sugar obtained by hydrolyzing wood with-hydrochloric acid are stirred up at ordinary temperature with 3 litres of a mixture containing 1 part of 95% 95 alcohol and 0.2 part of benzene together with 10 gms. of concentrated sulphuric acid; after standing a short while the whole is heated to and then the solvent is poured off; The latter. contains 30 gms; H01 and 31 guns. of 9 sugar, the sugar sugar and 0.3%
- What I claim is z 1.
- a process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid consisting in drying the wood sugar by atomization, removing the hydrochloric acid by-treating the resulting crude powder. with a solvent comprising an alcohol, converting the crude product into a syrup, and removing the solvent.
- a process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid consisting in drying the wood sugar by atomization, removing the hydrochloric acid by treating the resulting crude powder with a solvent comprising an alcohol,
- a process for purifying wood sugar obtained by hydrolyzing wood and other substances containingcellulose with hydrochloric acid consisting in drying the wood sugar by atomization, treating the loose crude powder obtained with a mixture of alcohol and benzene, converting the crude product into a syrup, and removing the solvent.
- a process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid consisting in drying the wood sugar by atomization, treating the loose crude powder obtained with a mixture of alcohol and benzene, sintering the crude product by gently heating the mixture, and removing the solvent.
- a process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid consisting in drying the wood sugar by atomization, treating the loose crude powder obtained With a mixture of 5 parts of 95% alcohol and 1 part of benzene, sintering the crude product by gently heating the mixture, and removing the solvent.
- a process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid consisting in' drying the wood sugar by atomization, treating the loose crude powder obtained with a mixture of 5 parts of 95% alcohol and 1 part of benzene, sintering the crude produce by heating the mixture to 50(50 (3., and removing the solvent.
- a process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid consisting in drying the wood sugar by atomization, treating the loose crude powder obtained with organic solvents containing oxygen which are capableof readily dissolving hydrochloric acid and which dissolve wood sugar with (lifliculty, and sintering the crude product and separating the solvent with the impurities by adding a small quantity of water to the mixture.
- a process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid consisting in drying the woodsugar by atomization, treating the loose crude powder obtained with a' mixture of alcohol and benzene, and sintering the crude product and separating the solvent with the impurities by adding a small quantity of water to the mixture.
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Patented June 21, 1932 UNITED STATES IPATENT OFFICE I EDUARD Fianna, or nnl nmnnne, enimauv, 'assrenon T iiOLZHYDIB/OLYSE Ax'rmu- GEBELLSCHAFT, or ntann snae, ennmmr pennies-non or'woon seem No Drawing. Application filed July 6, 1929,8eria1 No. 376,502,-
in Germany-July 7, 1928; l
Wood sugar, which is obtained by the hydrolysis of wood with concentrated hydrochloric acid, may be -freed, to a very large extent, from the excess hydrochloric acid if 5 the wood sugar solution in a finely atomized state is brought into contact with a hotcurrent of air '(see U. S. A. patent specification No. 1,678,819). The so-called dry-sugar obtained in this way still'posscsses two undesirable properties; it isa light, voluminous powder-consisting of particles of irregular shapes and large surfaces, which is therefore, ill-suited for transport and further working up, and also it contains resinous impurities 1 and always remnants of hydrochloric acid, which are detrimental for many purposes.
The removal of both of these disadvantages in a technically advantageous manner is the object of the invention. I I
2 It might be contemplated to wash out the impurities of the dry sugar withorganic solvents, such as alcohol, acetic anhydride and the like. The dry sugar, however, holds firmly in its pores large quantities of added nonaqueous liquids. Thus, 95% alcohol must be added in a quantity up to four times the Weight of the product before any of it drains oii. Moreover, even when still larger quantities of alcohol are 'used,'the alcohol draining off contains only very little of the hydrochloric acid which is present in the crude product to be purified. Only by washing out the alcohol retained bythe mass can considerable quantities of hydrochloric acid be brought into solution. However, it is not economical to work in this manner; the loss in sugar is considerable, the waste of alcohol is too great and its recovery too costly.,
According to the present invention, over 49 80% of the hydrochloric acid'present in the dry sugar can be separated by means of certain organic solvents by mere d'ecantation of the same from the sugar and simultaneously the sugar is converted into a syrup of high specific gravity. The organic solvents suitable for this purpose are organic liquids containing oxygen which dissolve hydrochloric acid readily and sugar with difficulty. They are soluble in water. The separation of sugar and hydrochloric acid may,
for instance, be attained by gently heating the mixture of'sugar and solvent.' The loose sugar thereby sinters together and the solvent used may then be easily and almost com.-
-pletely poured off. The degree of heating 6|! necessary dependson the. nature of the solvent and on its water content,
A mixture of 95 %'alcohol with benzene in the ratio of 5: 1 has proved to be particularly suitabld It is then suflicient to 'heat the mixture to 50--6 0. inorder to produce the desired sintering. The presence of benzene depresses the solubility of the sugar in alcohol and raises its absorption capability for the resinous extraneous constituents of the dry-sugar, I The separation of sugar and solvent and the simultaneous conversion of the sugar'into a syrup form may also be attained by adding a 7 small quantity of water to the mixture of sugar and aIeohoLbenZene. If the dry sugar werelfirst to be taken up with water and the syrup obtained treated with alcohol-benzene mixture, the original large surface of the dry sugar, otherwise firmly retaining the organic 75 solvent, would indeed be destoyed: however, at the same time, the partition coeflieient of the hydrogen chloride between the water in' the syrupand the organic solvent would be displaced in an unfavorable direction so so that much sugar would go into solution with but little hydrochloric acid. It would not be practical therefore to work in this manner. When the dry sugar contains chlorides besides free hydrochloric acid, it is of great 95 value to remove these chlorine ions also. This may be effected byadding fairly, a. small quantity of concentrated sulphuric acid to the solvent.
Ewamples 9 1. 1000 guns. of dry sugar obtained by hydrolyzing wood with-hydrochloric acid are stirred up at ordinary temperature with 3 litres of a mixture containing 1 part of 95% 95 alcohol and 0.2 part of benzene together with 10 gms. of concentrated sulphuric acid; after standing a short while the whole is heated to and then the solvent is poured off; The latter. contains 30 gms; H01 and 31 guns. of 9 sugar, the sugar sugar and 0.3%
present being calculated as hydrochloric acid), besides about 13% of water and 18.7% of alcohol mixed with benzene. Thus, about 2.8 litres of the solvent mixture used have been poured olf.
2. 1000 gms. of dry sugar obtained by bydrolyzing wood with hydrochloric acid are stirred up with 4 litresof the above mixture. After a short time, about 200 cc. of water are added in a finely divided state, whereupon the previously pulverized sugar goes over into syrup. The solvent contains 29 gms. .HCl and 40 gms. of sugar, and the syrup, 62% sugar and 0.3% HCl, besides about of water and 17.7% of alcohol-benzene. Thus,
' about 3.7 litres of the alcohol-benzene mix ture have been poured oil.
What I claim is z 1. A process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid, consisting in drying the wood sugar by atomization, removing the hydrochloric acid by-treating the resulting crude powder. with a solvent comprising an alcohol, converting the crude product into a syrup, and removing the solvent.
2. A process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid, consisting in drying the wood sugar by atomization, removing the hydrochloric acid by treating the resulting crude powder with a solvent comprising an alcohol,
sintering the crude product by gently heating the mixture, and removing the solvent.
3. A process for purifying wood sugar obtained by hydrolyzing wood and other substances containingcellulose with hydrochloric acid, consisting in drying the wood sugar by atomization, treating the loose crude powder obtained with a mixture of alcohol and benzene, converting the crude product into a syrup, and removing the solvent.
4. A process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid, consisting in drying the wood sugar by atomization, treating the loose crude powder obtained with a mixture of alcohol and benzene, sintering the crude product by gently heating the mixture, and removing the solvent.
5. A process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid,,consisting in drying the wood sugar by atomization, treating the loose crude powder obtained with a mixture of 5'parts of y 95% alcohol and 1 part of benzene, converting the crude product into a syrup,'and removlng the solvent.
6. A process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid, consisting in drying the wood sugar by atomization, treating the loose crude powder obtained With a mixture of 5 parts of 95% alcohol and 1 part of benzene, sintering the crude product by gently heating the mixture, and removing the solvent.
7. A process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid, consisting in' drying the wood sugar by atomization, treating the loose crude powder obtained with a mixture of 5 parts of 95% alcohol and 1 part of benzene, sintering the crude produce by heating the mixture to 50(50 (3., and removing the solvent.
8. A process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid, consisting in drying the wood sugar by atomization, treating the loose crude powder obtained with organic solvents containing oxygen which are capableof readily dissolving hydrochloric acid and which dissolve wood sugar with (lifliculty, and sintering the crude product and separating the solvent with the impurities by adding a small quantity of water to the mixture.
9. A process for purifying wood sugar obtained by hydrolyzing wood and other substances containing cellulose with hydrochloric acid, consisting in drying the woodsugar by atomization, treating the loose crude powder obtained with a' mixture of alcohol and benzene, and sintering the crude product and separating the solvent with the impurities by adding a small quantity of water to the mixture.
10. A process as claimed in claim 1 and in which a small quantity of concentrated sulphuric acid is added to the solvent.
In testimony whereof I havesigned my name to this specification.
EDUAR-D FARBER.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE1863654X | 1928-07-07 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US1863654A true US1863654A (en) | 1932-06-21 |
Family
ID=7746573
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US376502A Expired - Lifetime US1863654A (en) | 1928-07-07 | 1929-07-06 | Purification of wood sugar |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US1863654A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2959500A (en) * | 1956-02-14 | 1960-11-08 | Schweizerische Eidgenossenschaft | Process for the saccharification of cellulose and cellulosic materials |
| US20100044210A1 (en) * | 2008-08-20 | 2010-02-25 | The Board Of Regents Of The University Of Texas System | METHOD OF DIGESTING CELLULOSE TO GLUCOSE USING SALTS AND MICROWAVE (muWAVE) ENERGY |
| EP2620442A1 (en) | 2012-01-27 | 2013-07-31 | BIOeCON International Holding N.V. | Process for recovering saccharides from cellulose hydrolysis reaction mixture |
-
1929
- 1929-07-06 US US376502A patent/US1863654A/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2959500A (en) * | 1956-02-14 | 1960-11-08 | Schweizerische Eidgenossenschaft | Process for the saccharification of cellulose and cellulosic materials |
| US20100044210A1 (en) * | 2008-08-20 | 2010-02-25 | The Board Of Regents Of The University Of Texas System | METHOD OF DIGESTING CELLULOSE TO GLUCOSE USING SALTS AND MICROWAVE (muWAVE) ENERGY |
| EP2620442A1 (en) | 2012-01-27 | 2013-07-31 | BIOeCON International Holding N.V. | Process for recovering saccharides from cellulose hydrolysis reaction mixture |
| WO2013110814A1 (en) | 2012-01-27 | 2013-08-01 | Bioecon International Holding N.V. | Process for recovering saccharides from cellulose hydrolysis reaction mixture |
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