Method of hydrolytic decomposition of cellulose-containing raw material

专利摘要:
The invention relates to the hydrolysis industry and can be used for carrying out the processes of hydrolytic decomposition of various types of cellulosic raw materials. The purpose of the invention is to increase the yield and quality of sugar produced. The raw materials intended for hydrolysis treatment are crushed, impregnated with dilute sulfuric acid or another 0.5 to 10% acid solution, then mechanically dewatered to a moisture content of 10 to 80% and crushed again. / V i CO С 4 WITH со cm
公开号:SU1449013A3
申请号:SU823511352
申请日:1982-11-04
公开日:1988-12-30
发明作者:Хингер Клаус-Юрген
申请人:Вернер Унд Пфлейдерер (Фирма)；
IPC主号:

专利说明:

In loose form, the raw material is filled up in the pre-heating chamber 2 of the reactor 1, where it is heated to 100 ° C. After that, the material is sent to reactor 1. At the first stage of hydrolysis of raw materials in reactor 1, at 175 ° C and 0.9 MPa pressure, 40% of the cellulose is degraded. In the second stage, at 225 ° C and a pressure of 2.6 MPa, during 4.5 s, the degree of cellulose conversion rises from 4 to 30% and, finally, in the third stage at 260 ° C and a pressure of 4.8 MPa with a residence time of 1, 3 sec, the conversion is increased from 30% to 80%. After the third hydrolysis step in the reactor, the temperature and pressure are quickly reduced by expanding the steam. Lowering the temperature and pressure in the reaction volume of the reactor 1 is then also drained in three stages, respectively, to 225 ° C and 2.6 MPa, to 175 ° C and 0.9 MPa and to 100 ° C and 0.1 MPa for 2, 5 - 5 s. Simultaneously, steam is taken from all stages, retained, and used in the hydrolysis stages, and steam taken from the last stage of temperature and pressure reduction is used in the heating stage of the ground mass of raw material. The method of hydrolytic decomposition of cellulosic raw materials provides the possibility of increasing the yield and quality of the sugar produced. 5 il.
one
The invention relates to the hydrolysis industry and can be used for carrying out the processes of hydrolytic decomposition of various types of cellulosic raw materials.
The purpose of the invention is to increase the yield and quality of sugar produced.
FIG. 1 shows schematically an apparatus for carrying out the method of hydrolytically decomposing cellulose containing cf; in fig. 2 - diagram of the modes of the individual steps of the reaction; in fig. 3 — experimental dependencies of selectivity, degree of cellulose conversion and sugar yield on reaction time; Fig. 4 is a graph of selectivity to sugar versus cellulose conversion; in fig. 5 - dependence of specific steam consumption on the number of hydrolysis steps or steam tanks.
Device for hydrolytic. The decomposition of the cellulose-containing raw material contains a concave reaction vessel 1 made in the form of a high-pressure reactor. On the inner walls of vessel 1 there is an acid-resistant heat-conducting substance, for example, ceramics. Thermal insulation (not shown) is also provided in vessel 1. Above the reaction vessel is placed the preheating chamber 2. Chamber 2 is connected to rrlktor 1 using the inlet
five
0
30 5
The aperture 3 can be closed by the locking part of the moving valve 4 (in Fig. 1 it is shown in dotted position in the open position). The closing part of the valve 4 with the rod 5 and the hydraulic or pneumatic actuator 6 constitutes the inlet valve 7. Around the brush 5, cleaning devices 8 are provided for cleaning it from the remnants of the adhered processing material that are actuated by the hydraulic or pneumatic actuator 9.
In the lower part of the reaction vessel 1 there is an outlet 10, which is closed by the closing part of the valve 11 (in the open position in Fig. 1 is shown in dotted lines). The locking part 11 of the control rod 12 is connected to a hydraulic or pneumatic actuator 13. The control current 12 passes through the product discharge port 14 connected to the outlet 10. The locking part 11, the control plug 12 and the actuator 13 together form an outlet valve 14.
In the preheating chamber 2, on the side, there is a feed opening 15, to which a horizontal channel 16 abuts with a pusher 17 moving in a horizontal direction.
The funnel-shaped lower part 18 of the feed hopper 19 for the material is pushed into the channel 16 from the top.
In the reaction vessel 1 below the closing part 4 of the inlet valve 7, the annular nozzle channel 20 is located with a large number of steam injection nozzles 21. The annular nozzle channel 20 is connected to the output flat opening 22 and the exhaust steam pipe 23. From the exhaust vapor pipe 23 there is a pipeline 24 through the locking device 25 to the pre-heating chamber 2, while on the other hand the outlet steam pipe 23 is connected to the steam collectors 26 and 27 The steam collectors 26 and 27 belong to the locking devices 28 and 29.
The second annular nozzle channel 30 is located in the reaction vessel 1 above the closing part 11 of the outlet valve 14 and is connected to the steam inlet .31 and the supply steam pipe 32. The supply steam pipe 32 is connected to one side through the locking device 33, 34 or 35 a source of fresh pagch, not shown in figure 1, and on the other hand - with steam collectors 26 and 27.
The device works as follows.
The hopper 19 is filled with already-impregnated dehydrated and pulverized cellulose-containing material. The funnel-shaped lower part 18 and channel 16 act together as a dosed bath, which is limited to the right by the pusher 17 shown in FIG. 1 in the original position. With longitudinal movement of the pusher 17, the material is fed into the preheating chamber 2, while the inlet valve 7 is closed. In the final position, the pusher 17 closes the loading opening 15. No special requirements are imposed on the density of this unit.
Now, the preheating chamber 2, when the locking device 25 is opened, via pipe 24, steam comes from the last stage of the gap. The heat of condensation of the waste vapor is transferred to the material, which is heated to 100 C. After that, it opens4
five
with the inlet valve 7 and the material from the preheating chamber 2 in a loose form enters the reaction vessel 1 with the outlet valve 14 closed.
five


449013
ay ig d
0 on e 25
,
45
50
five
Due to the operation of the cleaning device 8, residual material is removed. When the inlet valve 7 is locked, the sealing surface can be cleaned with a steam jet. The cleaning devices 8 and the pusher 17 are thus returned to their original position and are then ready to repeat the loading process.
In the reaction vessel, a stepwise process of the hydrolytic decomposition of cellulose-containing flux begins. In the process of raw material hydrolysis, steam from steam collectors 26 and 27 is supplied one stage after another through feed pipe 32, and fresh steam through open shut-off device 33. The incoming steam passes through annular nozzle channel 30 so that the material subjected to hydrolysis is in fluidized bed.
After passing through the reactor stages, with stepwise expansion, the steam is led through the upper annular nozzle channel 20 and the conduit 23 to the steam collectors 26 and 27. The exhaust steam from the last expansion stage is fed through the shut-off device 25 into the preheating chamber 2. Therefore, the device is again ready to conduct a new cycle in quasi-continuous mode.
The method of hydrolytic decomposition of cellulosic raw materials is carried out on this device as follows.
The material to be hydrolyzed, for example, old paper, wood waste, straw, etc., is first crushed, then impregnated with dilute sulfuric acid or another suitable acid solution with a concentration of 0.5 to 10%, then mechanically dehydrated to moisture from 10 to 80% and then crushed again and loosely poured into the pre-heating chamber 2 of the reactor 1. Here the incoming material is heated to 100 ° C with the help of exhaust steam passed through the reaction stages, with e the condensation. After that, the material is directed to the reactor 1.
In the first stage of hydrolysis of the raw material in the reactor 1 at 175 ° C and a pressure of 0.9 MPa, up to 4% of cellulose is converted in 40 seconds. On the next
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FOR AND -.: M1-T. :. ur | ;; ui; h 1G1NR., |
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; , | : .a.; i ii-ip, required for an; 1 v:, i ML jpii.TTa when moving from sos-; g1in; 1 b p to match and to reach it iii in peiaKTope RH, is - :(. Pair, which is released- 14 C.-g. Then in d state s. Tak. .1. M, the second steam collector, can .. gt.on, n m7, superheated steam with parameter-, .M i |. J;; - l if-nyuspe expansion; 11 i jMen; HiiH of state d on state -, to kgishchestve, not: 10; 1dimom for
 n, .i from with. neither b g state d
I, :) needed to go from
 ..ig., gc to d and to increase the pressure; d.1; i, o g (. S; tg,. phenzhen come from steam-; mountain; fro the pressure must be biicoi-nif ,, n ppmrr 10 MPa to time; iyvjrsa (1T lv. 1vn to level d) f: h..t1, in comparison with Contin. L1.1 ;; H - 1 .10 POainiHH.
By.) ,, vihots shch.y with the last extension g :: flax,) th: 7 a: Uin after the change
; rt., downturn b to a level a is - ;; m 1, .sub.T Kahicpe 2 a preliminary -oi is a chagreva for heating a material, gannic acid. After the after-, i. li i I f - :. nbiu. r (3 heating can start 1, g. 1y rioaH iii reaction process.
ils figs, 1, lsduet that the specific p ..:. d pair dj required last i -:. ha and and heating, with an increase; h1,; ia and. l steam collectors and when;, - i .. v: tjHnii Bna; KH..jcTH injected for
p b i I lAH, ijpcjiingannogo cellulose soder-ftaiic ro material, is reduced.
As follows from FIG. 3, the dependence of ihohots of fermented sugar a, i.e. K04 i4t:; CTBa sugar, obtained from obr, chb, - pulverized cellulose, from the time of reaction has a maximum, which is from to; 1: - | The h-temperature temperature becomes higher and for a shorter period ;; ..- ripe Mc-iiii response. On fig.Z Louis 7 sin h temperature areas-. - three highs are relevant
. The degree of conversion of cellulose .1: ;; (: h; 1ts exponentially from 0% at. ii t vom vr.ts.1en.and stay up to 100%;.:;; long period of stay (t; i; c. see „fjHr ,, 3). Additional v upi. The division of selectivity S to fermentation, .1G; g, m: in sau.chru, i.e., the number of sugar- j; i .hischishees to the number of treatment- v, a, -f.; oH 1L} ozoi, led to build
(dependencies; presented on J, Hi of which implies that for i i:. ipiii bullet value of degree
14
conversion selectivity is about 100%
and further, as the conversion rate increases, it falls rapidly.
When the degree of conversion is t, the selectivity is 95% and at 260 ° C it is 90% and its decrease with an increase in the degree of conversion is slower. These phenomena can be explained by the existence of competing reactions at noBbmjeHHbix temperatures.
These experimental conclusions are based on the basic idea of the invention, which is that the maximum sugar yield can be obtained with a clock change in temperature. On the basis of the experimental data presented in FIG. 3, it can be concluded that the preferred stepwise implementation of the method as shown in FIG. 2. The method of hydrolytic decomposition of cellulose-containing raw materials provides the possibility of increasing the yield and quality of the sugar produced.

权利要求:
Claims (1)
[1]
Invention Formula
The method of hydrolytic decomposition of cellulosic raw materials, providing for acid treatment of the crushed mass of raw materials with 0.5-10%
138,
acid solution, its dehydration and subsequent hydrolysis with water vapor in several stages with an increase in pressure and temperature in the reaction volume at each stage, characterized in that, in order to increase the yield and quality of the sugar produced, the ground mass is dehydrated by 10-80% after dehydration is heated to 100 ° C, the number of hydrolysis stages is taken equal to three, and the temperature and pressure are increased at each stage respectively to 75 ° C pressure of 0.9 MPa for 40 s, to 225 C, pressure of 2.6 MPa for 4.5 s, up to 260 C, crushed 4.8 MPa for 1.3 s, while after the third stage of hydrolysis, a three-stage decrease in temperature and pressure in the reaction volume to 225 ° C and 26 MPa, respectively, to and up to 100 ° C and 0.1 MPa, respectively from 2.5 to 5 seconds, with simultaneous extraction of steam from all stages, its preservation and use at hydrolysis stages, and steam taken at the last stage of temperature and pressure lowering - at the stage of heating the crushed mass of raw material.
State
PLANT Sap
.% 7,260
1Q th 30 050 TOO ZOO 300 5OO
 pea / (t4ifu, t, with FIG. 3
Degrees euffpo usa.
I F
yo7o
07s
50% iOO%
 4e / i / tfo / to3t /,%
Phie.
0 1 Z sr ff Ko U ecfTj paroakumu / atoro
+
i 2 5 P 5 6 1 Ko / iui / ec / air defense eadro and a
Phie.
Uneconomical econoni1
Hufa / ibf affdo / fff bodb ffpofff / f me

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法律状态:

优先权:

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申请号 | 申请日 | 专利标题

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DE19813149587|DE3149587A1|1981-12-15|1981-12-15|METHOD AND DEVICE FOR HYDROLYTIC CLEAVING OF CELLULOSE|

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