专利摘要:
A method for producing xylans and fibrous materials by treating the xylan-containing feedstock with saturated water vapor at a temperature of 160-210 ° C and pressure, then processing the partially hydrolyzed feedstock with water and / or dilute alkali aqueous solution to produce an aqueous solution of xylanes and decomposition products xylans and water-insoluble residue - fibrous material, characterized in that, in order to increase the yield of the target products, the raw material is treated with steam for 5,240 m in at a pressure of 6.3-19.5 at. SP
公开号:SU1120924A3
申请号:SU772507802
申请日:1977-07-20
公开日:1984-10-23
发明作者:Херманн Дитрихс Ханс;Зиннер Михаель;Опдербек Фритц;Брахтхойзер Карл-Хайнц
申请人:Фритц Вернер Индустри Аусрюстунген Гмбх (Фирма);
IPC主号:
专利说明:

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This invention relates to an improved method for the production of xylans, fibrous materials and their cleavage products, which can be used as feed additives and building materials.
A known method for producing xylans, fibrous materials and products of their cleavage by treating a xylan-containing starting material with an aqueous alkali solution at 170-175 ° C. The degree of gaseous separation of the xylans is 25-30% l.
This method is not characterized by a high degree of xylan separation.
The closest to the technical essence of the proposed method is to obtain xylans, fibrous materials and their cleavage products by treating the xylan-containing feedstock with valuable steam at a temperature of 60-23Cf C and a pressure of 24.6-46 ppm for 1-2 minutes, processing partially progid-. Rolled with water and / or dilute aqueous solution of alkali to obtain an aqueous solution of xylans and products of the splitting of xylans and water-insoluble residue of fibrous material. The yield of the target products is 3-4% 2j.
The known method is characterized by an insufficiently high yield of ii; eJie products.
The purpose of the invention is to increase the yield of the target products.
This goal is achieved in that according to the method of producing xylans and fibrous materials by treating the xylan-containing starting material with saturated steam at a temperature of 160-210 ° C and pressure, then processing partially hydrolyzed with water and / or dilute aqueous alkali solution to produce an aqueous solution of xylans and the splitting products of xylans and the water-insoluble residue — fibrous material; treatment of the starting material with steam with water is carried out for 5–240 min at a pressure of 6.3-19.5 mp.
Example 1. 400 g of birch wood in the form of chips, which corresponds to 277 g of absolutely dry wood, treated in the laboratory
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refiner (firm Defibrator LZ) for 7 minutes with steam at 188 C, which corresponds to a pressure of about 12 MPa, and defibrated for 2 minutes. 5 The fibrous material is washed out of the defibrator with hot water and liquid is separated from the fibrous material in a hydraulic press. To the aqueous extract (3250 ml) is added
0 27 ml of sulfuric acid and for
60 minutes, the solution is heated in an autoclave to 120 C. Then the acidic filtrate is neutralized with a calculated amount of calcium hydroxide and sulphate precipitate.
5 Calcium is removed by centrifugation. After bleaching with activated carbon and filtering, the solution is concentrated by distillation under vacuum to a syrup, which is
0 is extracted 4 times - each time 250 ml - hot ethanol. The extracts mixed with ethanol are filtered and the solution is again concentrated by distillation under vacuum to a syrup of different condition. After seeding with a small amount of crystalline xylose and dispersion at a temperature of about 0 ° C, 7.2 g of crystalline xylose were obtained with
0 m.p. 144 ° C. A second crystallization of the mother liquor gives 6.6 g of crystalline xylose with a mp. 141 C. Xylose yield with respect to dry wood (absolutely dry) 5 wt.%.
Example 2. In a similar way as in example 1, 498 g of oat husk (absolutely dry) are treated. The first fraction of the crystalline xiQ vine is 22.5 g with a pl. 141 C, as a result of the second and third crystallization, 2.7 and 2.2 g of xylose were obtained, respectively. The yield of xylose relative to the dry matter
g (absolutely dry) 5.5 wt.%.
Example 3. Similarly, in example 1, treated with 306 g of wheat straw (completely dry). To remove contamination straw in
For 2 minutes, they are treated with a steam at a pressure of 12 atm and defibred for 1.5 minutes. After washing with water and removing water using a hydraulic press, the fibers are treated with steam for 16 min at pressure
12 ATI and defibrated 15s. In the first fraction, 20.2 g of crystalline xylose were obtained with a mp. 146 ° C. it
3
corresponds to a yield of 6.6% in relation to absolutely dry straw.
Example 4. 400 g of birch wood in the form of chips with a moisture content of 21%, i.e. 316 g of absolutely dry wood are treated in a laboratory refiner of the firm Defibrator AV for 80 minutes with steam at 185-190 ° C, which corresponds to a pressure of about 12 atm, and defibered for about 2 minutes. The wet fiber obtained in this way is washed out of the defibrator with a total volume of 4 liters of water and washed on a sieve. The yield of fibrous material is 193 g (61%) in relation to the used wood (absolutely dry) .. The fibrous material consists of approximately 37% of lignin (hydrolysis residue) and approximately 58% of carbohydrates. After hydrolysis of the fibrous material, the proportion of glucose in the total amount of carbohydrates is 91%. The analyzes are carried out as described in the preceding examples. Material absorption in ruminants is 79%.
The mixed wash water is concentrated under vacuum and the concentrate is freeze-dried. In this case, 63.4 g of material was obtained, which corresponds to a yield of 20.1% with respect to absolutely dry wood. This total dry matter content of the aqueous extract after hydrolysis contains 31 g of xylose (9.8% with respect to absolutely dry wood) and 23 g of other sugars.
Example 5. In another experiment, carried out under other identical conditions as in Example 1, the processing time was extended to 120 minutes. The yield of fibrous material is 190 g (60% relative to the wood used, completely dry). The fibrous material consists of about 35% lignin (hydrolysis residue) and about 58% of carbohydrates with glucose content of 93%. The digestibility of the material in ruminants is 80%.
The freeze-dried wash water contains 51.5 g of dry matter, which corresponds to a yield of 16.3% with respect to wood (absolutely dry). This dry substance after hydrolysis contains 16 g of xylose (5.1% with respect to wood.
244
absolutely cyxoii) and 12 g of other sugars.
Examples 6-12. In each case, 395 g of airborne pulpwood, which corresponds to 300 g of absolutely dry wood, is processed according to the conditions specified in example 1 with saturated steam at a pressure of 12 atm.
and a temperature of 187 C for the time shown in the table, and the resulting fibrous materials are extracted with water according to Example 1. Contained in the fibrous material
the cellulose is hydrolyzed to glucose, and exclusively pure glucose is obtained. The table shows the quantities of the substance obtained in each case, with the numbers in brackets indicating the quantity in relation to the starting material (absolutely dry). Aqueous extracts contain polymeric and oligomeric products.
cleavage of xylans, the number of which is also indicated in the table. These products have a molecular weight in the range of 300-6000. About high purity of polymeric and oligomeric
the xylans cleavage products can be judged by the fact that when they are converted to xylose, the yield of the latter relative to them is 87% by weight. Example 13. 100 g of finely chopped straw, which corresponds to 90 g of absolutely dry straw, are treated in a laboratory refiner (Defibrator AV company) with steam for 60 minutes at a temperature of 170 C, pressure is 8.1 atm and defibrated for 1 minute. The obtained wet fibrous material is washed out of the defibrator with water (4 liters) and washed on a sieve. The yield of fibrous material 54 g (60%)
; relation to the used straw (absolutely dry). The fibrous material consists of about 24% lignin (hydrolysis residue) and as a result of hydrolysis, 76% of carbohydrates are obtained with glucose content of 85% (35 g). The analyzes are carried out as described in the preceding examples. The digestibility of fibrous material in ruminants 68%.
The wash water collected together is concentrated and freeze-dried. The yield of dry matter 30 g (33%) relative to the
straw (absolutely dry). After hydrolysis of the dry substance, 18.3 g (61%) of carbohydrates were obtained with a xylose content of 14.3 g (78% in relation to the obtained carbohydrates and 15.9% in relation to straw, absolutely dry).
Example 14. 200 g of freshly chopped birch wood, which makes 139 g of absolutely dry wood in the form of chips, are treated for 5 minutes with steam at a temperature of 210 ° C and a pressure of 19.5 atm and in accordance with example 1 are split into fibers and extracted with water. The yield of fibrous material is 96 g (69%) with respect to recovered wood (absolutely dry). Total fiber content
the carbohydrate material after hydrolysis is 64%, of which 85% (52 g) of glucose. The digestibility of the fibrous material in ruminants, tested in accordance with Example 4, is 61%.
Example 15. When processing in example 1 of birch wood at a temperature of 160 C and a pressure of 6.3 MPa
over 4 hours, 97 g (70%) of fibrous material is obtained. The total carbohydrate content after hydrolysis is 65%, of which 87% (55 g) of glucose. Absorbability of fibrous material
63%.
The use of the invention allows to increase the yield of target products to 81.4%.
权利要求:
Claims (1)
[1]
METHOD FOR PRODUCING XYLANES AND FIBROUS MATERIALS by treating a xylan-containing feedstock with saturated steam at a temperature of 160-210 ° C and pressure, followed by treating the partially hydrolyzed feedstock with water and / or a dilute aqueous alkali solution to obtain an aqueous solution of xylans and xylene and insoluble degradation products water residue - fibrous material, characterized in that, in order to increase the yield of target products, the processing of the feedstock with water vapor is carried out for 5 - §
240 min at a pressure of 6.3-19.5 bar.
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1 1120924
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同族专利:
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法律状态:
优先权:
申请号 | 申请日 | 专利标题
AT534676A|AT361506B|1976-07-20|1976-07-20|METHOD FOR OBTAINING XYLAN AND FIBER FIBERS FROM VEGETABLE RAW MATERIALS CONTAINING XYLAN|
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