CN114713134A - Gas-solid method for producing cellulose mixed ether - Google Patents
Gas-solid method for producing cellulose mixed ether Download PDFInfo
- Publication number
- CN114713134A CN114713134A CN202210324962.7A CN202210324962A CN114713134A CN 114713134 A CN114713134 A CN 114713134A CN 202210324962 A CN202210324962 A CN 202210324962A CN 114713134 A CN114713134 A CN 114713134A
- Authority
- CN
- China
- Prior art keywords
- pipe
- reaction kettle
- gear
- box body
- tank
- 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.)
- Pending
Links
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000001913 cellulose Substances 0.000 title claims abstract description 59
- 229920002678 cellulose Polymers 0.000 title claims abstract description 57
- 239000007787 solid Substances 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 39
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims abstract description 110
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims abstract description 102
- 238000006243 chemical reaction Methods 0.000 claims abstract description 99
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims abstract description 67
- 238000000034 method Methods 0.000 claims abstract description 45
- 239000000463 material Substances 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 238000000926 separation method Methods 0.000 claims abstract description 19
- 238000006266 etherification reaction Methods 0.000 claims abstract description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 229920000742 Cotton Polymers 0.000 claims abstract description 4
- 229920001131 Pulp (paper) Polymers 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000002386 leaching Methods 0.000 claims abstract description 4
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 4
- 238000011085 pressure filtration Methods 0.000 claims abstract description 4
- 238000007670 refining Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000005540 biological transmission Effects 0.000 claims description 44
- 239000007788 liquid Substances 0.000 claims description 42
- 230000001360 synchronised effect Effects 0.000 claims description 41
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
- 238000005057 refrigeration Methods 0.000 claims description 23
- 229940050176 methyl chloride Drugs 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- 238000007599 discharging Methods 0.000 claims description 16
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 9
- 230000007246 mechanism Effects 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 6
- 230000001276 controlling effect Effects 0.000 claims description 5
- 230000000149 penetrating effect Effects 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 3
- 230000002093 peripheral effect Effects 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- FBBDOOHMGLLEGJ-UHFFFAOYSA-N methane;hydrochloride Chemical compound C.Cl FBBDOOHMGLLEGJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 239000003507 refrigerant Substances 0.000 description 100
- 235000010980 cellulose Nutrition 0.000 description 39
- 239000007789 gas Substances 0.000 description 15
- 238000009835 boiling Methods 0.000 description 7
- 239000002826 coolant Substances 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 230000000670 limiting effect Effects 0.000 description 5
- 229920003086 cellulose ether Polymers 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 241000270295 Serpentes Species 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003780 insertion Methods 0.000 description 3
- 230000037431 insertion Effects 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000009191 jumping Effects 0.000 description 2
- 229920003124 powdered cellulose Polymers 0.000 description 2
- 235000019814 powdered cellulose Nutrition 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a gas-solid method production process of cellulose mixed ether, which comprises the following steps: crushing: crushing cotton pulp or wood pulp; alkalization and etherification: adding powdery cellulose, alkali liquor, chloromethane, ethylene oxide and dimethyl ether into a reaction kettle, heating to 40-70 ℃ at a constant speed, and carrying out alkalization etherification reaction; neutralizing: after the reaction is finished, separating and recovering the unreacted chloromethane, ethylene oxide and dimethyl ether, and adding hydrochloric acid into the residual materials for neutralization; refining: and after neutralization, adding water into the materials for washing, filtering, leaching and steam pressure filtration by a continuous washing centrifugal filter, and finally crushing and drying to obtain the finished product cellulose mixed ether. According to the invention, the auxiliary stirring device is added in the reaction kettle, so that the stirring efficiency is improved, and the cellulose alkalization etherification efficiency is further improved. And the chloromethane, the ethylene oxide and the dimethyl ether which participate in the reaction are separated, recovered and recycled through a separation device.
Description
Technical Field
The invention belongs to the technical field of production of cellulose mixed ether, and particularly relates to a gas-solid production process of cellulose mixed ether.
Background
Cellulose mixed ether refers to ether with two substituent groups with different properties on the molecular chain of cellulose ether. Because the properties of two different cellulose ethers are combined, the cellulose ether can more comprehensively and completely exert the properties of the cellulose ether, has better solubility, dispersibility, transparency, enzyme resistance, salt resistance and the like than single ether, and is widely applied to a plurality of industrial fields and daily life.
The production technology of cellulose mixed ether mainly includes two methods of gas-solid method and solid-liquid method (solvent method). The gas-solid method process is that during etherification, ethylene oxide, chloromethane and a certain amount of dimethyl ether which are used as etherifying agents are injected into a reaction kettle after being pressurized into liquid state, and then the liquid is directly reacted with alkali cellulose.
In the existing gas-solid method process, methyl chloride, ethylene oxide and dimethyl ether are consumed greatly, and some unreacted substances are also wasted in other forms after being emptied, so that the substances cannot be fully utilized.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the invention overcomes the defects of the prior art and provides a gas-solid method production process of cellulose mixed ether. And the chloromethane, the ethylene oxide and the dimethyl ether which participate in the reaction are separated, recovered and recycled through a separation device.
The technical scheme adopted by the invention for solving the problems in the prior art is as follows:
the gas-solid production process of cellulose mixed ether comprises the following steps:
A. crushing: crushing cotton pulp or wood pulp to obtain powdery cellulose with the particle size of 200-230 mu m and the bulk density of 180-200 g/L;
B. alkalization and etherification: adding powdery cellulose and alkali liquor into a reaction kettle, injecting high-pressure nitrogen into the reaction kettle for boosting the pressure to 2.3MPa, adding high-pressure liquid chloromethane, ethylene oxide and dimethyl ether, raising the temperature to 40-70 ℃ at a constant speed, and carrying out alkalization etherification reaction;
C. neutralizing: after the reaction is finished, the pressure of the reaction kettle is relieved, and unreacted chloromethane, ethylene oxide and dimethyl ether are gasified and discharged into a separation device for separation and recovery; discharging the residual materials out of the reaction kettle, and then adding hydrochloric acid for neutralization to maintain the pH value of the materials between 6 and 8;
D. refining: and after neutralization, adding water into the materials for washing, filtering, leaching and steam pressure filtration by a continuous washing centrifugal filter, and finally crushing and drying to obtain the finished product cellulose mixed ether.
Preferably, the reaction kettle in the step B comprises a reaction kettle tank body with an open upper end, and a reaction kettle upper cover and a stirring paddle which are covered above the reaction kettle tank body.
The bottom of the reaction kettle body is provided with a discharge hole, and the discharge hole is provided with a valve.
The top of the upper cover of the reaction kettle is connected with a first feeding pipe, a second feeding pipe, a boosting pipe and a pressure relief pipe in a run-through manner.
A stop valve is arranged on the first feeding pipe.
The second feeding pipe is respectively connected with a chloromethane supply pipeline, an ethylene oxide supply pipeline and a dimethyl ether supply pipeline through valves.
The pressure rising pipe is connected with a nitrogen supply pipeline.
The pressure relief pipe is communicated with the separating device.
The stirring rake includes the oar axle, and the oar axle is coaxial to be set up in the internal portion of reation kettle jar, is fixed with the paddle on the oar axle, and the oar axle upper end is worn to establish to the outside of reation kettle upper cover and is fixed with first conical gear.
A first motor is fixed on the upper cover of the reaction kettle and drives the first star-chasing gear to rotate.
Preferably, the reaction kettle tank body is sequentially provided with a cylindrical area, a circular truncated cone area and a discharging pipe from top to bottom, wherein the cylindrical area, the circular truncated cone area and the discharging pipe are coaxially arranged, the vertical section of the circular truncated cone area is in a circular truncated cone shape, the diameter of the upper end of the circular truncated cone area is larger than that of the lower end of the circular truncated cone area, the inner diameter of the discharging pipe is the same as that of the lower end of the circular truncated cone area, and the inner diameter of the cylindrical area is the same as that of the upper end of the circular truncated cone area.
And a gate valve is arranged at the opening at the lower end of the blanking pipe.
The paddle shaft is tubular, a central shaft coaxially penetrates through the paddle shaft, an annular supporting plate is sleeved on the circumferential surface of the central shaft and located in the circular platform area, and the lower end of the paddle shaft is rotatably connected with the supporting plate
The circumference surface of the central shaft below the supporting plate is wound with a spiral sheet, the spiral sheet is inserted in the blanking pipe, and the outer diameter of the spiral sheet is the same as the inner diameter of the blanking pipe.
The upper end of the central shaft penetrates through the outer part of the upper cover of the reaction kettle and is fixed with a second bevel gear.
The first motor output shaft drives the second bevel gear to rotate.
Preferably, the lower end of the central shaft is fixed with a bottom shaft, a ring groove is concavely arranged on the circumferential surface of the bottom shaft, a lantern ring is rotatably sleeved inside the ring groove, and the circumferential surface of the lantern ring is fixedly connected with the inner wall of the blanking pipe through a plurality of fixing rods.
Preferably, the inner wall of the tank body of the reaction kettle is provided with a toothed ring.
A plurality of auxiliary stirring devices distributed in an annular array around the axis of the tank body are arranged in the tank body of the reaction kettle.
The auxiliary stirring device comprises a rotating shaft, blades and a first gear, wherein one end of the rotating shaft is inserted into the paddle shaft or the inner wall of the paddle, and the other end of the rotating shaft is fixedly connected with the first gear.
A plurality of blades are fixedly connected with the circumferential surface of the rotating shaft
The pivot is connected with oar axle or paddle rotation, and first gear sets up on the ring gear, and first gear is connected with the ring gear meshing.
Preferably, a driving mechanism is arranged above the upper cover of the reaction kettle.
The driving mechanism comprises a first transmission rod, a second transmission rod, a third transmission rod, a fourth transmission rod, a fifth transmission rod and a regulating device.
The first transmission rod comprises a third bevel gear and a first belt pulley which are coaxially and fixedly connected through a rotating rod.
The second transmission rod comprises a fourth bevel gear, a second belt pulley and a third belt pulley which are coaxially and fixedly connected through a rotating rod.
The third transmission rod comprises a driven gear, a fourth belt pulley, a second gear and a third gear which are coaxially and fixedly connected through a rotating rod.
The fourth transmission rod comprises a fifth belt pulley and a fourth gear which are coaxially and fixedly connected through a rotating rod.
The fifth transmission rod comprises a sixth belt pulley and a fifth gear which are coaxially and fixedly connected through a rotating rod.
The regulating and controlling device comprises a second telescopic rod, a vertical rod, an upper roller and a lower roller, wherein the second telescopic rod, the vertical rod, the upper roller and the lower roller are vertically arranged, the lower end of the vertical rod is fixedly connected with the top end of the telescopic part of the second telescopic rod, the upper roller and the lower roller are respectively arranged on two sides of the vertical rod from top to bottom, and the axis of the upper roller and the axis of the lower roller are horizontally arranged.
The third bevel gear is meshed with the second bevel gear, and the first belt pulley is connected with the fifth belt pulley through a first synchronous belt.
The fourth bevel gear is meshed with the first bevel gear, the second belt pulley is connected with the fourth belt pulley through a second synchronous belt, and the third belt pulley is connected with the sixth belt pulley through a third synchronous belt.
The vertical rod is arranged between the second synchronous belt and the third synchronous belt, the upper roller is positioned right above the second synchronous belt, and the lower roller is positioned right below the third synchronous belt.
When the upper roller is not in contact with the second synchronous belt, the second synchronous belt is in a loose state.
When the lower roller is not in contact with the third synchronous belt, the third synchronous belt is in a loose state.
The driven gear is meshed with a driving gear on an output shaft of the first motor, the second gear is meshed with the fifth gear, and the third gear is meshed with the fourth gear.
Preferably, the separation device comprises three liquefaction tanks, and the three liquefaction tanks are respectively used for liquefying ethylene oxide, methyl chloride and dimethyl ether.
The liquefaction case include first box, the inner chamber of first box is the cuboid, is equipped with snake shape refrigeration pipe in first box length direction's the inner wall, the exit of snake shape refrigeration pipe is worn to establish to first box outside and in refrigerating unit's pipeline through connection.
The outside intake pipe and the blast pipe rather than inner chamber through connection that are equipped with of first box, first bottom of the case portion indent has the flowing back recess, and flowing back recess bottom through connection has the fluid-discharge tube, and the fluid-discharge tube end is worn to establish to first box outside.
A valve is arranged on the liquid discharge groove or the liquid discharge pipe.
And an air inlet pipe of a liquefaction box for liquefying the ethylene oxide is communicated with a pressure relief pipe of the reaction kettle.
The exhaust pipe of the liquefaction box for liquefying the ethylene oxide is communicated with the air inlet pipe of the liquefaction box for liquefying the chloromethane.
The exhaust pipe of the liquefied chloromethane liquefaction box is communicated with the air inlet pipe of the liquefied dimethyl ether liquefaction box.
The exhaust pipe of the liquefaction tank for liquefying the dimethyl ether is communicated with the nitrogen recovery pipeline.
Preferably, the first box is internally and vertically provided with a piston, and the peripheral end faces of the piston are abutted against the inner wall of the first box.
At least two screw rods are arranged inside the first box body along the length direction, the screw rods penetrate through the piston and are in threaded connection with the piston, one end of each screw rod is inserted into the inner wall of the first box body, and the other end of each screw rod penetrates through the first box body and is fixedly connected with a seventh belt pulley.
The second motor is fixed to the outside of the first box, an eighth belt pulley is fixed to an output shaft of the second motor, and the eighth belt pulley is connected with all the seventh belt pulleys through the same fourth synchronous belt.
Preferably, the air inlet pipe and the air outlet pipe are connected with the side wall of one end of the first box body in the length direction.
The side wall of the other end of the first box body in the length direction is provided with a through hole.
And a rubber sleeve is fixed at one end of the piston facing the through hole and is in threaded connection with the screw.
Preferably, the outer part of the liquefaction box is provided with a gas box, and the gas box comprises a second box body with an open upper end.
An elastic sealing gasket is arranged at an opening above the second box body in a covering mode and is fixedly connected with the second box body through a fixing frame.
The outside through connection of second box has the chemical examination pipe, is equipped with the stop valve on the chemical examination pipe, the through-hole through connection air flue and second box through connection.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method adopts one-step alkalization etherification reaction, adopts constant temperature rise in the reaction process, and has better etherification substitution uniformity and more uniform and stable product properties compared with the two-stage temperature rise of the conventional process.
(2) A certain amount of dimethyl ether is added as an inhibitor in the alkalization etherification reaction process, so that the reaction is more uniform, the occurrence of side reaction is inhibited, and the utilization rate of an etherifying agent is improved.
(3) The rotating shaft of the auxiliary stirring device in the reaction kettle is perpendicular to the rotating shaft of the stirring paddle, so that the flowing condition of materials in the reaction kettle is changed, the stirring efficiency is improved, and the alkalization etherification efficiency of cellulose is improved.
(4) The equal-diameter spiral piece is arranged in the discharging pipe, discharging is carried out through the spiral piece, and the discharging effect is better.
(5) The unreacted chloromethane, ethylene oxide and dimethyl ether are recovered and separated by a separation device and then are utilized.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a partial flow chart of the gas-solid method production process of cellulose mixed ether of the invention,
FIG. 2 is a flow chart of a refrigerating system in the gas-solid method production process of cellulose mixed ether of the invention,
FIG. 3 is a view showing the appearance of a reaction vessel in the production process of the cellulose mixed ether by the gas-solid method of the invention,
FIG. 4 is an exploded view of a reaction kettle in the gas-solid method production process of cellulose mixed ether of the present invention,
figure 5 is an enlarged view of a portion of figure 4 at a,
FIG. 6 is a first sectional view of a reaction vessel in the gas-solid method production process of cellulose mixed ether of the present invention,
FIG. 7 is a second sectional view of the reaction vessel in the gas-solid method production process of cellulose mixed ether of the present invention,
figure 8 is an enlarged view of a portion of figure 7 at B,
FIG. 9 is a horizontal sectional view of a feeding pipe of a reaction kettle in the production process of the cellulose mixed ether by the gas-solid method of the invention,
FIG. 10 is a horizontal cross-sectional view of a gate valve of a reaction kettle in the gas-solid method production process of cellulose mixed ether of the invention,
figure 11 is a longitudinal cross-sectional view of figure 9,
figure 12 is an enlarged view of a portion of figure 11 at C,
FIG. 13 is a structural diagram of a stirring paddle and a driving mechanism of a reaction kettle in the production process of the cellulose mixed ether by the gas-solid method of the invention,
FIG. 14 is a schematic view of a stirring paddle of a reaction kettle in the production process of the cellulose mixed ether by the gas-solid method of the invention,
FIG. 15 is a schematic view of the driving mechanism of the reaction kettle in the production process of the cellulose mixed ether by the gas-solid method of the invention,
FIG. 16 is a first outline view of a separating device in the production process of the cellulose mixed ether by the gas-solid method of the invention,
FIG. 17 is a second outline drawing of a separating device in the production process of the cellulose mixed ether by the gas-solid method of the invention,
FIG. 18 is an exploded view of the gas box of the separation device in the gas-solid method production process of cellulose mixed ether of the present invention,
FIG. 19 is a sectional view of the outer shell of the liquefaction tank in the separation device in the production process of the cellulose mixed ether by the gas-solid method of the invention,
figure 20 is an enlarged view of a portion of figure 19 at D,
FIG. 21 is a sectional view of a liquid level sensor of a liquid tank in the separation device in the production process of the cellulose mixed ether by the gas-solid method of the invention,
FIG. 22 is a sectional view of a piston of a liquefaction tank in the separation device in the production process of the cellulose mixed ether by the gas-solid method of the invention,
FIG. 23 is a schematic view of the cooling pipe inside the liquefaction box in the separation apparatus in the gas-solid method production process of cellulose mixed ether of the present invention,
FIG. 24 is a diagram showing the connection effect of the piston and its driving mechanism of the liquefaction tank in the separation device in the gas-solid method production process of cellulose mixed ether according to the present invention.
In the figure: 1-reaction kettle tank body, 101-discharge pipe, 1011-lantern ring, 1012-fixing rod, 102-valve body, 1021-slot, 103-circular table area, 2-reaction kettle upper cover, 201-first feed pipe, 202-second feed pipe, 203-pressure rising pipe, 204-pressure releasing pipe, 3-propeller shaft, 301-paddle, 302-first bevel gear, 4-auxiliary stirring device, 401-rotating shaft, 402-blade, 403-first gear, 5-gear ring, 501-spacing ring, 6-spiral sheet, 601-bottom shaft, 602-ring groove, 603-central shaft, 604-second bevel gear, 605-supporting plate, 7-inserting plate, 701-first telescopic rod, 8-first motor, 801-driving gear, 9-a first transmission rod, 901-a third bevel gear, 902-a first pulley, 10-a second transmission rod, 1001-a fourth bevel gear, 1002-a second pulley, 1003-a third pulley, 11-a third transmission rod, 1101-a driven gear, 1102-a fourth pulley, 1103-a second gear, 1104-a third gear, 12-a fourth transmission rod, 1201-a fifth pulley, 1202-a fourth gear, 13-a fifth transmission rod, 1301-a sixth belt pulley, 1302-a fifth gear, 14-a regulation and control device, 1401-a second telescopic rod, 1402-a vertical rod, 1403-an upper roller, 1404-a lower roller, 15-a first synchronous belt, 16-a second synchronous belt, 17-a third synchronous belt and 18-a protective cover;
19-a first box body, 1901-a guide rod, 1902-a through hole, 1903-a liquid drainage groove, 1904-a through cavity, 20-a piston, 2001-a rubber sleeve, 21-a screw, 2101-a seventh belt pulley, 22-a second motor, 2201-an eighth belt pulley, 2202-a fourth synchronous belt, 23-a snake-shaped refrigerating pipe, 24-an air inlet pipe, 25-an exhaust pipe, 26-a lifting valve, 27-a liquid drainage pipe and 28-an electronic liquid level meter;
29-air box, 2901-second box, 2902-elastic sealing gasket, 2903-fixing frame, 2904-assay tube, 30-connecting air channel;
31-nitrogen tank, 32-intermediate tank, 33-storage tank, 34-common refrigerating unit, 35-standby refrigerating unit, 36-temperature sensor and 37-electric control three-way valve;
01-nitrogen inlet pipe, 02-nitrogen return pipe, 03-connecting gas pipe, 04-first liquid collecting pipe, 05-second liquid collecting pipe, 06-first liquid inlet pipe, 07-second liquid inlet pipe and 08-third liquid inlet pipe;
001-low temperature box refrigerant discharge pipe, 002-refrigerant recycling pipe, 003-high temperature box refrigerant inlet pipe, 004-high temperature box refrigerant discharge pipe, 005-common unit refrigerant return pipe, 006-low temperature box refrigerant supply pipe, 007-low temperature box refrigerant bypass discharge pipe, 008-standby unit refrigerant discharge pipe, 009-high temperature box standby refrigerant supply pipe, 0011-high temperature box standby refrigerant return branch pipe, 0012-high temperature box refrigerant total return pipe, 0013-standby unit refrigerant return pipe, 0014-low temperature box standby refrigerant supply header pipe, 0015-low temperature box standby refrigerant supply branch pipe and 0016-low temperature box standby refrigerant return pipe.
Detailed Description
As used in the specification and in the claims, certain terms are used to refer to particular components. As one skilled in the art will appreciate, manufacturers may refer to a component by different names. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, that a person skilled in the art will be able to solve the technical problem within a certain error range, substantially to achieve the technical result.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", horizontal ", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The following will explain the production process of cellulose mixed ether by gas-solid method in more detail with reference to the attached drawings, but the invention is not limited thereto.
The gas-solid method production process of the cellulose mixed ether comprises the following steps:
A. crushing: cellulose pulp such as cotton pulp or wood pulp is crushed to obtain powdery cellulose with the particle size of 200-230 mu m and the bulk density of 180-200 g/L.
B. Alkalization and etherification: adding powdery cellulose and alkali liquor into a reaction kettle, injecting high-pressure nitrogen into the reaction kettle to increase the pressure to 2.3MPa, adding high-pressure liquid methyl chloride, ethylene oxide and dimethyl ether, heating to 40-70 ℃ at a constant speed, in the embodiment, heating to 70 ℃ at a constant speed, heating for 1.5h, keeping the temperature for 1.5h, and carrying out alkalization etherification reaction;
the raw material mixture ratio is that powdered cellulose: methyl chloride: ethylene oxide: alkali liquor: in this example, the weight of powdered cellulose, chloromethane, ethylene oxide, alkali solution (50 wt% sodium hydroxide solution) and dimethyl ether are respectively as follows: 2650kg, 1860kg, 400kg, 4000kg and 1600 kg.
C. Neutralizing: after the reaction is finished, the pressure of the reaction kettle is relieved, and unreacted chloromethane, ethylene oxide and dimethyl ether are gasified and discharged into a separation device for separation and recovery. Discharging the residual materials out of the reaction kettle, and then adding hydrochloric acid for neutralization to maintain the pH value of the materials between 6 and 8; or continuously keeping the material in the reaction kettle, and adding hydrochloric acid into the reaction kettle for neutralization to ensure that the pH value of the material is 7 +/-1.
D. Refining: after neutralization, adding 8 times of 90 ℃ hot water by mass into the materials for washing, then filtering, leaching and steam pressure filtration are carried out by a continuous washing centrifugal filter, and finally crushing and drying are carried out to obtain the finished product of cellulose mixed ether.
In the step B, the alkalization etherification efficiency of the cellulose and the chloromethane, the ethylene oxide and the dimethyl ether are influenced by the stirring efficiency of the reaction kettle, but the stirring paddle of the existing stirring kettle, whether the stirring paddle is of a paddle type, a flap paddle type, an anchor type, a frame type, a push type or a straight blade turbine type, only rotates around a paddle shaft, so that the material flow in the reaction kettle has a certain rule, and more materials cannot be impacted, so that the contact and reaction probability among different materials is reduced, and the alkalization etherification efficiency in the reaction kettle is further influenced.
In order to improve the reaction efficiency of the reaction kettle, the reaction kettle is optimally designed in the embodiment.
The reaction kettle in the step B of the embodiment comprises a reaction kettle tank body 1 with an open upper end, and a reaction kettle upper cover 2 and a stirring paddle which are arranged above the reaction kettle tank body 1 in a covering manner.
The discharge gate is equipped with to the 1 bottom of the reactor tank body, and discharge gate department is equipped with the valve, and reation kettle adopts vertically, and the discharge gate is under, is favorable to arranging the material.
Be equipped with the intensification pipeline in the 1 inside of reation kettle jar body, the inside circulation oil heat conduction oil of pipeline, the pipeline is connected with outside heat conduction oil heating device, heats the 1 inside of reation kettle jar body through high temperature heat conduction oil. Or an electric heating piece is added in the inner wall of the reaction kettle tank body 1 to heat the interior of the reaction kettle tank body 1 by generating heat.
In order to further facilitate the blanking, the reaction kettle tank body 1 is provided with a cylindrical area, a circular truncated cone area 103 and a blanking pipe 101 which are coaxially arranged from top to bottom. The cylindrical area and the blanking pipe 101 are both cylindrical. The vertical section of the circular truncated cone area 103 is in a circular truncated cone shape with the diameter of the upper end larger than that of the lower end, the inner diameter of the blanking tube 101 is the same as that of the lower end of the circular truncated cone area 103, and the inner diameter of the cylindrical area is the same as that of the upper end of the circular truncated cone area 103.
The lower end opening of the blanking pipe 101 is provided with a gate valve, and the gate valve comprises a valve body 102, a gate 7 and a first telescopic rod 701. The middle of the valve body 102 is a through hole with the same diameter as the blanking pipe 101, a slot 1021 is inwards recessed on the circumferential surface of the through hole, and half of the slot 1021 is communicated with the outer wall of the valve body 102. The insertion plate 7 is inserted into the insertion slot 1021, and the end surface of the insertion plate 7 exposed to the outside of the valve body 102 is fixedly connected with the tail end of the telescopic part of the first telescopic rod 701. The first extension rod 701 is fixed to the outer wall of the valve body 102.
The first telescopic rod 701 is an electric telescopic rod and adopts the prior art. The telescopic part extends to drive the inserting plate 7 to slide out of the slot 1021, so that a through hole in the middle of the valve body 102 is opened, and blanking can be performed; the telescopic part is shortened, the inserting plate 7 is driven to be inserted into the inserting groove 1021, and the through hole in the middle of the valve body 102 is blocked.
The top of the reaction kettle upper cover 2 is connected with a first feeding pipe 201, a second feeding pipe 202, a pressure boosting pipe 203 and a pressure relief pipe 204 in a penetrating way.
A stop valve is arranged on the first feeding pipe 201 and is used for adding powdery cellulose and alkali liquor under the normal pressure state;
the second feeding pipe 202 is respectively connected with a methyl chloride supply pipeline, an ethylene oxide supply pipeline and a dimethyl ether supply pipeline through valves, a one-way valve is connected on the second feeding pipe 202 in series, and the one-way valve ensures that materials can only be added into the reaction kettle through the second feeding pipe 202;
the booster pipe 203 is connected with a nitrogen supply pipeline, and the booster pipe 203 is also provided with a one-way valve;
the pressure relief pipe 204 is connected to the separator, and is also provided with a check valve.
The stirring paddle comprises a vertical paddle shaft 3, the paddle shaft 3 is coaxially arranged in the reaction kettle tank body 1, the paddle shaft 3 is fixedly provided with a paddle 301, and the paddle 301 is in a frame type or an anchor type. The upper end of the paddle shaft 3 penetrates through the outer part of the reaction kettle upper cover 2 and is fixed with a first bevel gear 302.
The paddle shaft 3 is tubular, a central shaft 603 coaxially penetrates through the paddle shaft 3, an annular supporting plate 605 is sleeved on the circumferential surface of the central shaft 603, the supporting plate 605 is located in the circular platform area 103, and the lower end of the paddle shaft 3 is rotatably connected with the supporting plate 605.
The circumferential surface of the central shaft 603 below the supporting plate 605 is wound with the spiral sheet 6, the spiral sheet 6 is inserted into the discharging pipe 101, the outer diameter of the spiral sheet 6 is the same as the inner diameter of the discharging pipe 101, that is, the outer wall of the spiral sheet 6 contacts with the inner wall of the discharging pipe 101. The height of the spiral sheet 6 is higher than the blanking pipe 101, i.e. a part of the spiral sheet 6 is located inside the circular truncated cone region 103.
The upper end of the central shaft 603 penetrates the outer part of the upper cover 2 of the reaction kettle and is fixed with a second bevel gear 604.
The lower end of the central shaft 603 is fixed with a bottom shaft 601, a circular groove 602 is concavely arranged on the circumferential surface of the bottom shaft 601, a sleeve ring 1011 is rotatably sleeved inside the circular groove 602, and the circumferential surface of the sleeve ring 1011 is fixedly connected with the inner wall of the blanking pipe 101 through a plurality of fixing rods 1012. The distance between the bottom surface of the bottom shaft 601 and the inserting plate 7 is less than 1 cm.
A plurality of auxiliary stirring devices 4 distributed in an annular array around the axis of the tank body 1 are arranged in the tank body of the reaction kettle.
The auxiliary stirring device 4 includes a rotating shaft 401, a blade 402 and a first gear 403, wherein one end of the rotating shaft 401 is inserted into the inner wall of the paddle shaft 3 or the paddle 301, and the other end is fixedly connected with the first gear 403. Several blades 402 are fixed on the circumference of the shaft 401, and the blades 402 can be rod-shaped, straight plate or curved plate.
The rotating shaft 401 is rotatably connected with the paddle shaft 3 or the paddle 301.
The inner wall of the reactor tank body 1 is provided with a gear ring 5 which is fixedly connected with the same shaft, a first gear 403 is arranged on the gear ring 5, and the first gear 403 is meshed with the gear ring 5. The rotating stirring paddle drives the rotating shaft 401 to rotate around the axis of the paddle shaft 3, and further drives the first gear 403 to move along the gear ring 5. Because the first gear 403 is meshed with the gear ring 5, the first gear 403 can roll and rotate on the gear ring 5 to drive the blades 402 to rotate, so as to stir the materials in the reaction kettle. Make inside the device that has two kinds of rotation directions difference simultaneously of reation kettle like this for can produce the striking when reation kettle inside material flows, and then increase reaction efficiency.
In order to avoid the first gear 403 from jumping, a limiting ring 501 is arranged right above the gear ring 5, the limiting ring 501 is fixedly connected with the inner wall of the reaction kettle tank 1 through welding or bolt connection and the like, the first gear 403 is located between the gear ring 5 and the limiting ring 501, and the limiting ring 501 blocks the first gear 403 from jumping upwards.
A first motor 8 and a driving mechanism are fixed on the reaction kettle upper cover 2.
The drive mechanism comprises a first drive rod 9, a second drive rod 10, a third drive rod 11, a fourth drive rod 12, a fifth drive rod 13 and a control device 14.
The first transmission rod 9 comprises a third bevel gear 901 and a first belt pulley 902 which are coaxially and fixedly connected through a rotating rod;
the second transmission rod 10 comprises a fourth bevel gear 1001, a second belt pulley 1002 and a third belt pulley 1003 which are coaxially and fixedly connected through a rotating rod;
the third transmission rod 11 comprises a driven gear 1101, a fourth belt pulley 1102, a second gear 1103 and a third gear 1104 which are coaxially and fixedly connected through a rotating rod;
the fourth transmission rod 12 comprises a fifth belt pulley 1201 and a fourth gear 1202 which are coaxially and fixedly connected through a rotating rod;
the fifth transmission rod 13 comprises a sixth belt pulley 1301 and a fifth gear 1302 which are coaxially and fixedly connected through a rotating rod;
the adjusting and controlling device 14 comprises a second extension bar 1401, a vertical bar 1402, an upper roller 1403 and a lower roller 1404, which are vertically arranged. The second telescopic rod 1401 adopts the electric prior art, the lower end of the vertical rod 1402 is fixedly connected with the top end of the telescopic part of the second telescopic rod 1401, the upper roller 1403 and the lower roller 1404 are respectively arranged at the two sides of the vertical rod 1402 from top to bottom, and the axes of the upper roller 1403 and the lower roller 1404 are horizontally arranged.
The third bevel gear 901 is engaged with the second bevel gear 604, and the first pulley 902 and the fifth pulley 1201 are connected by a first timing belt 15.
The fourth bevel gear 1001 is engaged with the first bevel gear 302, the second pulley 1002 is connected with the fourth pulley 1102 through the second timing belt 16, and the third pulley 1003 is connected with the sixth pulley 1301 through the third timing belt 17.
The vertical rod 1402 is disposed between the second timing belt 16 and the third timing belt 17, the upper roller 1403 is located directly above the second timing belt 16, and the lower roller 1404 is located directly below the third timing belt 17.
When the upper roller 1403 is not in contact with the second timing belt 16, the second timing belt 16 is in a relaxed state; when the lower roller 1404 is not in contact with the third timing belt 17, the third timing belt 17 is in a slack state.
The driven gear 1101 is engaged with a drive gear 801 on an output shaft of the first motor 8, the second gear 1103 is engaged with a fifth gear 1302, and the third gear 1104 is engaged with a fourth gear 1202.
The first motor 8 drives the driving gear 801 to rotate, and in order to control the rotation speed of the driving gear 801, the first motor 8 adopts a speed reduction motor, or a speed reduction box is additionally arranged between the first motor 8 and the driving gear 801.
The driving gear 801 rotates the driven gear 1101, and then the third transmission rod 11 rotates the fourth transmission rod 12 and the second transmission rod 10 through the second timing belt 16. The fourth transmission rod 12 drives the first transmission rod 9 to rotate through the first synchronous belt 15. The first transmission rod 9 drives the screw plate 6 to rotate, and the second transmission rod 10 drives the propeller shaft 3 to rotate, so as to drive the rotating shaft 401 to rotate.
When materials in the reaction kettle are stirred, the rotating direction of the driving gear 801 is unchanged, and at the moment, the rotating direction of the spiral piece 6 enables the materials to move from the blanking pipe 101 to the circular truncated cone area 103, so the materials cannot flow into the gate valve. Meanwhile, a part of the spiral sheet 6 is positioned in the circular platform area 103 and is contacted with the reaction materials, so that the spiral sheet can drive the materials from bottom to top to play a certain stirring role.
Under the condition that the rotation direction of the driving gear 801 is kept unchanged, the tightness states of the second synchronous belt 16 and the third synchronous belt 17 are changed by controlling the extension and retraction of the extension and retraction part of the second telescopic rod 1401, the rotation direction of the second transmission rod 10 is adjusted, the forward and reverse rotation of the propeller shaft 3 is changed, and the stirring efficiency in the reaction kettle is further improved.
Since the second gear 1103 is engaged with the fifth gear 1302, the third transmission rod 11 and the fifth transmission rod 15 rotate in opposite directions.
When the telescopic part of the second telescopic rod 1401 moves downwards, the upper roller 1403 presses the second synchronous belt 16 downwards, the lower roller 1404 is far away from the third synchronous belt 17, the second synchronous belt 16 is tightened, and the third synchronous belt is loosened, so that the third transmission rod 11 drives the second transmission rod 10 to rotate, and the paddle shaft 3 is driven to rotate towards one direction; on the contrary, when the extension part of the second extension rod 1401 moves upwards, the upper roller 1403 is separated from the second synchronous belt 16, the lower roller 1404 presses the third synchronous belt 17, the second synchronous belt 16 is loosened, and the third synchronous belt is tightened, so that the fifth transmission rod 13 drives the second transmission rod 10 to rotate, and the paddle shaft 3 is driven to rotate towards another direction. Therefore, by controlling the operation of the second extension bar 1401, the rotation direction of the propeller shaft 3 can be adjusted without changing the rotation direction of the first motor 8.
When discharging is needed, the second telescopic rod 1401 controls the upper roller 1403 and the lower roller 1404 not to be contacted with the two conveying belts, the first motor 8 rotates reversely, and the spiral sheet 6 drives the material to move below the discharging pipe 101 and discharge the material. The inner wall of the circular platform area 103 is an inclined surface, so that the blanking is more facilitated.
And in the step C, separating and recovering unreacted chloromethane, ethylene oxide and dimethyl ether by adopting a normal-pressure condensation mode. To achieve this, the present embodiment envisages a separating device.
The separation device comprises three liquefaction tanks, wherein the three liquefaction tanks are respectively used for liquefying ethylene oxide, chloromethane and dimethyl ether, the boiling point of the ethylene oxide is 10.8 ℃, the boiling point of the chloromethane is-24.2 ℃ and the boiling point of the dimethyl ether is-29.5 ℃ under normal pressure. Thus, ethylene oxide is liquefied and separated, methyl chloride is separated, and dimethyl ether is separated.
The liquefaction case include first box 19, the inner chamber of first box 19 is the cuboid, and the vertical cross-sectional shape on its width direction is the square. A snake-shaped refrigerating pipe 23 is arranged in the inner wall of the first box body 19 in the length direction, and an inlet and an outlet of the snake-shaped refrigerating pipe 23 penetrate through the first box body 19 and are connected with a pipeline of a refrigerating unit in a penetrating way.
An air inlet pipe 24 and an exhaust pipe 25 which are communicated with the inner cavity of the first box body 19 are arranged outside the first box body 19, a liquid discharge groove 1903 is concavely arranged at the bottom of the first box body 19, a liquid discharge pipe 27 is communicated with the bottom of the liquid discharge groove 1903, and the tail end of the liquid discharge pipe 27 penetrates through the first box body 19.
A valve is disposed on the drainage groove 1903 or the drainage pipe 27, and in this embodiment, a lift valve 26 is disposed inside the drainage groove 1903. The lift valve 26 is lowered to close the through connection between the drain recess 1903 and the drain pipe 27, and the lift valve 26 is entirely located inside the drain recess 1903.
In order to carry out liquid level monitoring, the inside chamber 1904 that link up is equipped with of the lateral wall of first box 19 and intake pipe 24, link up chamber 1904 upper and lower both sides all with the inside through hole through connection of first box 19, link up the inside electron level gauge 28 that is equipped with perpendicularly of chamber 1904.
The air inlet pipe 24 of the liquefaction box for liquefying the ethylene oxide is communicated with the pressure relief pipe 204 of the reaction kettle; an exhaust pipe 25 of a liquefaction tank for liquefying ethylene oxide is communicated with an intake pipe 24 of a liquefaction tank for liquefying chloromethane; an exhaust pipe 25 of a liquefied methane chloride tank is communicated with an intake pipe 24 of a liquefied dimethyl ether tank; an exhaust pipe 25 of a liquefaction tank for liquefying dimethyl ether is communicated with the nitrogen recovery pipeline.
The intake pipe 24 and the exhaust pipe 25 are connected to a side wall of one end of the first case 19 in the longitudinal direction, that is, the through-hole is located on the side wall of one end of the first case 19 in the longitudinal direction. A through hole 1902 is provided in a side wall of the other end of the first case 19 in the longitudinal direction.
The piston 20 is vertically arranged in the first box body 19, the peripheral end faces of the piston 20 are abutted to the inner wall of the first box body 19, and the piston 20 divides the interior of the first box body 19 into two independent chambers.
At least two screws 21 are arranged in the first box 19 along the length direction, the screws 21 penetrate through the piston 20, the screws 21 are in threaded connection with the piston 20, one end of each screw 21 is inserted into the inner wall of the first box 19, and the other end of each screw 21 penetrates through the outer part of the first box 19 and is fixedly connected with a seventh belt pulley 2101.
The second motor 22 is fixed outside the first box 19, an eighth belt pulley 2201 is fixed on an output shaft of the second motor 22, and the eighth belt pulley 2201 is connected with all the seventh belt pulleys 2101 through a same fourth synchronous belt 2202.
In this embodiment, two screws 21 are symmetrically arranged around the center of the piston 20, and the second motor 22 drives the two screws 21 to rotate at the same time, so that the two screws 21 are synchronous, thereby preventing the piston 20 from jamming during the moving process.
In order to further improve the smoothness of the movement of the piston 20, a horizontally arranged guide rod 1901 is fixed between two side surfaces of the first box 19 in the length direction, the axis of the guide rod 1901 is parallel to the axis of the screw 21, and the guide rod 1901 penetrates through the piston 20.
To improve the sealing, a sliding seal is provided between the piston 20 and the guide rod 1901.
A rubber sleeve 2001 is fixed to one end of the piston 20 facing the through hole 1902, and the rubber sleeve 2001 is screwed to the screw 21. The rubber sleeve 2001 has elasticity, and thus it can be brought into close contact with the screw 21, improving the sealing property.
The inner wall of the first box 19 which is connected with the air inlet pipe 24 and the air outlet pipe 25 in a penetrating way is embedded with a pressure sensor, and the pressure sensor monitors the pressure inside a space on one side of the piston 20 facing the air inlet pipe 24 and the air outlet pipe 25 in real time. When gas enters the first box 19 and the pressure is increased, the piston 20 moves towards the through hole 1902 to increase the space and reduce the internal pressure; when part of the gas liquefies and the pressure decreases, the piston 20 moves in the direction of the intake pipe 24, decreasing the space and increasing the internal pressure.
The outer part of the liquefaction box is provided with an air box 29, the air box 29 comprises a second box body 2901 with the upper end open, an opening above the second box body 2901 is covered with an elastic sealing gasket 2902, and the elastic sealing gasket 2902 is fixedly connected with the second box body 2901 through a fixing frame 2903.
The second box 2901 is externally connected with a test tube 2904, the test tube 2904 is provided with a stop valve, and the through hole 1902 is connected with the second box 2901 through a connecting air passage 30. The piston 20 is moved by the gas in the gas box 29, and the elastic packing 2902 is used to elastically change the inner space of the second box 2901, and is matched with the movement of the piston 20.
The addition of the air tank 29 connects the three first tanks 19 to form a closed space in which the pistons 20 are directed toward the through-holes 1902, so that ethylene oxide, methyl chloride and dimethyl ether flow only inside the space even though they pass through the pistons 20.
The test tube 2904 is then periodically evacuated to test the contents of ethylene oxide, methyl chloride and dimethyl ether in the space to assess the tightness of the piston 20, as is known in the art. Air may be supplied to the air box 29 through the test tube 2904.
The refrigeration unit is prior art, and this embodiment adopts the refrigeration unit the same with the air conditioner principle, includes motor, compressor, relevant pipeline and inside refrigerant promptly.
The system formed by the reaction kettle and the separation device further comprises a nitrogen tank 31, an intermediate tank 32, a storage tank 33 and an electric cabinet, wherein the electric cabinet adopts the prior art and comprises a control device and a power module, the control device adopts a PLC or an integrated circuit with an industrial control chip, and all electric devices inside the whole system are electrically connected with the electric cabinet.
The export of nitrogen gas jar 31 is connected with reation kettle's the pipe 203 that steps up through nitrogen gas intake pipe 01, and it has booster pump and stop valve to establish ties on the nitrogen gas intake pipe 01, to the inside high-pressure nitrogen gas that injects into of reation kettle, plays the guard action promptly, blows off the inside air of reation kettle totally, also can increase the inside pressure of reation kettle simultaneously, realizes the effect of pressure boost.
The air inlet pipe 24 of the liquefaction box for liquefying the ethylene oxide is communicated with the pressure relief pipe 204 of the reaction kettle through a connecting air pipe 03; an exhaust pipe 25 of a liquefied ethylene oxide tank is communicated with an air inlet pipe 24 of a liquefied chloromethane tank through a connecting air pipe 03; an exhaust pipe 25 of a liquefied chloromethane tank is communicated with an air inlet pipe 24 of a liquefied dimethyl ether tank through a connecting air pipe 03; the exhaust pipe 25 of the liquefaction tank for liquefying dimethyl ether is connected with the nitrogen tank 31 through a nitrogen return pipe 02.
The liquid discharge pipes 27 of the three liquefaction tanks are all connected to the separate intermediate tank 32 through the first collection pipe 04, and the intermediate tank 32 is connected to the separate storage tank 33 through the second collection pipe 05. The first liquid collecting pipe 04 and the second liquid collecting pipe 05 are both connected in series with a booster pump and a stop valve.
The three storage tanks 33 are used for storing high-pressure liquefied ethylene oxide, methyl chloride and dimethyl ether, respectively.
The three storage tanks 33 are respectively connected with the first feed pipe 201 through a first liquid inlet pipe 06, a second liquid inlet pipe 07 and a third liquid inlet pipe 08, and a booster pump and a stop valve are connected in series on the first liquid inlet pipe 06, the second liquid inlet pipe 07 and the third liquid inlet pipe 08.
The connecting air pipe 03 and the nitrogen return air pipe 02 can be connected with an air pump and a stop valve in series, and air in the previous container is pumped into the next container by the air pump.
Gas transfer may also be achieved in another form. Namely, after the alkalization etherification is completed, the pressure relief pipe 204 is opened firstly, the pressure in the reaction kettle is reduced, and the ethylene oxide, the chloromethane and the dimethyl ether are gasified. Then, nitrogen gas under normal pressure was injected into the reaction vessel, and ethylene oxide, methyl chloride and dimethyl ether in the reaction vessel were blown out through a pressure relief pipe and blown into a liquefaction tank for liquefying ethylene oxide.
The refrigerating unit reduces the temperature in the liquefaction box for liquefying the ethylene oxide to-20 ℃ to 10 ℃, the piston 20 is moved to adjust the air pressure in the space where the mixed gas is located, so that the air pressure is kept at about normal pressure, the ethylene oxide in the internal mixer starts to liquefy, the internal air pressure is reduced in the liquefying process, and the internal pressure is kept by adjusting the position of the piston 20.
After the refrigeration time reaches the threshold value, or the height of the electronic liquid level meter is not changed, and meanwhile, when the detection data of the pressure sensor are not changed, the lifting valve 26 is opened, the liquefied ethylene oxide is pressurized and pumped into the intermediate tank 32, the high-pressure liquefied ethylene oxide is stored in the intermediate tank 32, and when the storage amount of the internal ethylene oxide reaches the threshold value, the liquefied ethylene oxide is pumped into the storage tank 33 of the ethylene oxide.
After all the liquefied ethylene oxide is discharged, the piston 20 is moved in the direction of the exhaust pipe 25 to push out the gas remaining in the first tank 19 and into the liquefaction tank for liquefying methyl chloride through the connecting pipe 3. The refrigerating unit reduces the temperature in the liquefaction box for liquefying the methyl chloride to-28 ℃ to-25 ℃, liquefies the methyl chloride in the mixed gas, and pumps the liquefied methyl chloride into the independent middle pipe. After all the liquid is discharged, the piston 20 is moved to push the remaining gas into the liquefaction tank for liquefying dimethyl ether.
The refrigerating unit reduces the temperature inside the liquefaction tank for liquefying dimethyl ether to below-30 ℃, liquefies and separates the dimethyl ether inside the mixed gas, and pumps the dimethyl ether into the independent intermediate tank 32.
Then, the piston 20 is moved to push the remaining nitrogen gas into the nitrogen gas tank 31, and the nitrogen gas is reused. And (4) performing sampling inspection on gas components in the nitrogen tank 31 at regular time, and detecting the contents of ethylene oxide, chloromethane and dimethyl ether in the nitrogen tank.
Because the boiling point of the ethylene oxide is 10.8 ℃, the boiling point of the methyl chloride is-24.2 ℃, the boiling point of the dimethyl ether is-29.5 ℃, and the boiling point of the ethylene oxide is more than 30 ℃ higher than that of the methyl chloride and the dimethyl ether, in order to save energy consumption, in the embodiment, as shown in the attached figure 2, two common refrigerating units 34 are arranged to respectively refrigerate the liquefaction tanks of the methyl chloride and the dimethyl ether, meanwhile, two snake-shaped refrigerating pipes 23 are respectively arranged inside two opposite side walls in the width direction of the liquefaction tank of the ethylene oxide, and the outlets of the snake-shaped refrigerating pipes of the liquefaction tanks of the methyl chloride and the dimethyl ether are respectively communicated with the inlets of the two snake-shaped refrigerating pipes 23 inside the liquefaction tank of the ethylene oxide. The coolant cools the liquefaction tank of methyl chloride and dimethyl ether earlier, then inside the snake refrigeration pipe 23 that flows into the ethylene oxide liquefaction case, utilizes the waste heat to carry out temperature regulation at the ethylene oxide liquefaction case.
That is, the two common refrigerating units 34 inject liquid refrigerants into the snake-shaped refrigerating pipe 23 inside the liquefaction box of methyl chloride and dimethyl ether through the low-temperature box refrigerant supply pipe 006, the refrigerants reduce the temperature inside the first box 19 in the methyl chloride and dimethyl ether liquefaction boxes, then the refrigerants are discharged through the low-temperature box refrigerant discharge pipe 001, the refrigerants are discharged into the snake-shaped refrigerating pipe 23 inside the ethylene oxide liquefaction box, the temperature inside the ethylene oxide liquefaction box is adjusted, and then the refrigerants flow back to the interior of the common refrigerating unit 34 through the common unit refrigerant return pipe 005 to refrigerate, and the next circulation is started.
However, after the coolant cools the chloromethane liquefaction tank, the dimethyl ether liquefaction tank, or the chloromethane and dimethyl ether liquefaction tank, the temperature of the coolant may be too high, and the ethylene oxide liquefaction tank cannot be cooled continuously. In this case, in order to maintain the temperature of the ethylene oxide liquefaction tank, the backup refrigerator group 35 is added in the present embodiment. Meanwhile, related connecting pipelines are optimally designed.
At this time, a temperature sensor 36 is provided on the cryotank refrigerant discharge pipe 001 for detecting the temperature of the refrigerant inside the cryotank refrigerant discharge pipe 001, an electrically controlled three-way valve 37 is provided at the end of the cryotank refrigerant discharge pipe, and three joints of the electrically controlled three-way valve 37 are connected to the cryotank refrigerant discharge pipe 001, the refrigerant recycling pipe 002, and the cryotank refrigerant bypass discharge pipe 007, respectively.
The end of the refrigerant recycling pipe 002 is connected with a refrigerant inlet pipe 003 of the high-temperature box and a standby refrigerant supply pipe 009 of the high-temperature box through an electric control three-way valve.
The end of the low-temperature tank refrigerant bypass discharge pipe 007 is connected with a common unit refrigerant return pipe 005 through a valve.
The outlets of two snake-shaped refrigeration pipes 23 in the ethylene oxide liquefaction box are communicated with a high-temperature box refrigerant discharge pipe 004, and the tail end of the high-temperature box refrigerant discharge pipe 004 is connected with a common unit refrigerant backflow pipe 005 and a high-temperature box refrigerant main backflow pipe 0012 through an electric control three-way valve.
The high-temperature tank refrigerant main return pipe 0012 and the high-temperature tank standby refrigerant supply pipe 009 are respectively in through connection with the refrigerant inlet and outlet of the standby refrigerating unit 35.
When the temperature sensor 36 detects that the temperature of the refrigerant inside the low-temperature tank refrigerant discharge pipe 001 is higher than the threshold value and cannot reduce the temperature inside the ethylene oxide liquefaction tank to be lower than 10.8 ℃, the corresponding electrically-controlled three-way valves 37 all adjust the paths for the refrigerant to flow. At this time, the refrigerant inside the low-temperature tank refrigerant discharge pipe 001 flows into the low-temperature tank refrigerant bypass discharge pipe 007 through the electrically controlled three-way valve, then flows into the common unit refrigerant return pipe 005, and finally enters the common refrigeration unit 34 for cooling. The backup refrigeration unit 35 is started to flow the low-temperature refrigerant inside the backup refrigeration unit into the refrigerant liquid inlet pipe 003 of the high-temperature tank through the backup refrigerant supply pipe 009 of the high-temperature tank and the electric control three-way valve, and the temperature inside the ethylene oxide liquefaction tank is reduced inside the serpentine refrigeration pipe 23 flowing into the ethylene oxide liquefaction tank. The refrigerant after heat exchange flows back to the inside of the standby refrigerating unit 35 through the high-temperature tank refrigerant discharge pipe 004, the electric control three-way valve and the high-temperature tank refrigerant main return pipe 0012, and is cooled again.
The backup refrigerating unit 35 can not only be used for refrigerating the ethylene oxide liquefaction box, but also be used as a backup unit to replace any one common refrigerating unit 34 when one of the two common refrigerating units 34 is in failure shutdown. Some necessary piping is added for this purpose.
That is, the refrigerant outlet of the backup refrigeration unit 35 is connected to the backup unit refrigerant discharge pipe 008, and the end of the backup unit refrigerant discharge pipe 008 is connected to the high-temperature tank backup refrigerant supply pipe 009 and the low-temperature tank backup refrigerant supply header 0014, respectively, through the electrically controlled three-way valve.
The main coolant supply line 0014 for the low-temperature tank is connected to two branch coolant supply lines 0015 for the low-temperature tank through two valves, and the two branch coolant supply lines 0015 for the low-temperature tank supply the low-temperature coolant to the liquefaction tanks for methyl chloride and dimethyl ether.
The end of the low-temperature tank backup refrigerant supply branch 0015 is connected with the low-temperature tank refrigerant supply pipe 006 through a valve, and the low-temperature tank backup refrigerant supply branch 0015 is connected with the common refrigeration unit 34 in parallel.
The refrigerant inlet of the standby refrigerating unit 35 is in through connection with a refrigerant return pipe 0013 of the standby unit, and the other end of the refrigerant return pipe 0013 of the standby unit is connected with a main refrigerant return pipe 0012 of the high-temperature box and a standby refrigerant return pipe 0016 of the low-temperature box through an electric control three-way valve.
The other end of the backup refrigerant return pipe 0016 of the low-temperature tank is connected with a refrigerant bypass discharge pipe 007 of the low-temperature tank and a refrigerant return pipe 005 of the common unit through an electric control three-way valve.
When one of the conventional refrigerating units 34 fails, the flow path of the refrigerant becomes: the system comprises a standby refrigerating unit 35, a standby unit refrigerant discharge pipe 008, a low-temperature tank standby refrigerant supply header pipe 0014, a low-temperature tank standby refrigerant supply branch pipe 0015, a low-temperature tank refrigerant supply pipe 006, a dimethyl ether liquefaction tank or a chloromethane liquefaction tank, a low-temperature tank refrigerant discharge pipe 001, a low-temperature tank refrigerant bypass discharge pipe 007, a low-temperature tank standby refrigerant return pipe 0016, a standby unit refrigerant return pipe 0013 and a standby refrigerating unit 35, wherein the standby refrigerating unit refrigerant discharge pipe is connected with the low-temperature tank standby refrigerant supply branch pipe 0015;
or, the backup refrigerating unit 35, the backup unit refrigerant discharge pipe 008, the low-temperature tank backup refrigerant supply header pipe 0014, the low-temperature tank backup refrigerant supply branch pipe 0015, the low-temperature tank refrigerant supply pipe 006, the dimethyl ether liquefaction tank or the methyl chloride liquefaction tank, the low-temperature tank refrigerant discharge pipe 001, the refrigerant reuse pipe 002, the ethylene oxide liquefaction tank, the high-temperature tank refrigerant discharge pipe 004, the high-temperature tank refrigerant main return pipe 0012, the backup unit refrigerant return pipe 0013, and the backup refrigerating unit 35.
Because the two serpentine refrigeration circuits 23 are independent within the ethylene oxide liquefaction tank, they are conveniently connected to a common refrigeration unit 34, but are not readily connected to a backup refrigeration unit 35. In order to refrigerate the ethylene oxide liquefaction case alone when practical reserve refrigerating unit 35, two snakelike refrigeration pipe 23 are inside can both to let in the refrigerant, supply the branch pipe through the reserve refrigerant of automatically controlled three-way valve connection high-temperature box between two high-temperature box refrigerant feed liquor pipes 003 in this embodiment, through the reserve refrigerant backward flow branch pipe 0011 of automatically controlled three-way valve connection high-temperature box between two high-temperature box refrigerant discharge pipes 004. By adjusting the valve core position of the electric control three-way valve, the two snake-shaped refrigeration pipes 23 inside the ethylene oxide liquefaction box are connected into a whole by the warm box standby refrigerant supply branch pipe and the high temperature box standby refrigerant backflow branch pipe 0011, so that the standby refrigeration unit 35 can simultaneously inject refrigerants into the two snake-shaped refrigeration pipes 23.
The embodiments of the present invention have been described in detail with reference to the drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention.
Claims (10)
1. The gas-solid method production process of the cellulose mixed ether is characterized by comprising the following steps:
A. crushing: crushing cotton pulp or wood pulp to obtain powdery cellulose with the particle size of 200-230 mu m and the bulk density of 180-200 g/L;
B. alkalization and etherification: adding powdery cellulose and alkali liquor into a reaction kettle, injecting high-pressure nitrogen into the reaction kettle for boosting, increasing the pressure to 2.3MPa, adding high-pressure liquid chloromethane, ethylene oxide and dimethyl ether, raising the temperature to 40-70 ℃ at a constant speed, and carrying out alkalization etherification reaction;
C. neutralizing: after the reaction is finished, the pressure of the reaction kettle is relieved, and unreacted chloromethane, ethylene oxide and dimethyl ether are gasified and discharged into a separation device for separation and recovery; discharging the residual materials out of the reaction kettle, and then adding hydrochloric acid for neutralization to maintain the pH value of the materials between 6 and 8;
D. refining: and after neutralization, adding water into the material for washing, filtering, leaching and steam pressure filtration by a continuous washing centrifugal filter, and finally crushing and drying to obtain the finished product cellulose mixed ether.
2. The gas-solid method production process of cellulose mixed ether according to claim 1, characterized in that:
the reaction kettle in the step B comprises a reaction kettle tank body (1) with an opening at the upper end, and a reaction kettle upper cover (2) and a stirring paddle which are covered above the reaction kettle tank body (1),
a discharge hole is arranged at the bottom of the reaction kettle tank body (1), a valve is arranged at the discharge hole,
the top of the upper cover (2) of the reaction kettle is connected with a first feeding pipe (201), a second feeding pipe (202), a pressure boosting pipe (203) and a pressure relief pipe (204) in a run-through way,
a stop valve is arranged on the first feeding pipe (201),
the second feeding pipe (202) is respectively connected with a methyl chloride supply pipeline, an ethylene oxide supply pipeline and a dimethyl ether supply pipeline through valves,
the booster pipe (203) is connected with a nitrogen gas supply pipeline,
the pressure relief pipe (204) is communicated with the separating device,
the stirring paddle comprises a paddle shaft (3), the paddle shaft (3) is coaxially arranged in the reaction kettle tank body (1), a paddle blade (301) is fixed on the paddle shaft (3), the upper end of the paddle shaft (3) penetrates through the outer part of the reaction kettle upper cover (2) and is fixed with a first conical gear (302),
a first motor (8) is fixed on the upper cover (2) of the reaction kettle, and the first motor (8) drives a first star wheel gear (302) to rotate.
3. The gas-solid method production process of cellulose mixed ether according to claim 2, characterized in that:
the reaction kettle tank body (1) is sequentially provided with a cylindrical area, a circular truncated cone area (103) and a discharging pipe (101) which are coaxially arranged from top to bottom, the vertical section of the circular truncated cone area (103) is in a circular truncated cone shape, the diameter of the upper end of the circular truncated cone area is larger than that of the lower end of the circular truncated cone area, the inner diameter of the discharging pipe (101) is the same as that of the lower end of the circular truncated cone area (103), the inner diameter of the cylindrical area is the same as that of the upper end of the circular truncated cone area (103),
a gate valve is arranged at the opening at the lower end of the blanking pipe (101),
the paddle shaft (3) is tubular, a central shaft (603) coaxially penetrates through the paddle shaft (3), an annular supporting plate (605) is sleeved on the circumferential surface of the central shaft (603), the supporting plate (605) is positioned in the circular platform area (103), the lower end of the paddle shaft (3) is rotatably connected with the supporting plate (605),
the circumferential surface of the central shaft (603) below the supporting plate (605) is wound with a spiral sheet (6), the spiral sheet (6) is inserted into the blanking pipe (101), the outer diameter of the spiral sheet (6) is the same as the inner diameter of the blanking pipe (101),
the upper end of the central shaft (603) is arranged outside the upper cover (2) of the reaction kettle in a penetrating way and is fixed with a second bevel gear (604),
an output shaft of the first motor (8) drives the second bevel gear (604) to rotate.
4. The gas-solid method production process of cellulose mixed ether according to claim 3, characterized in that:
the lower end of the central shaft (603) is fixed with a bottom shaft (601), a circular groove (602) is concavely arranged on the circumferential surface of the bottom shaft (601), a sleeve ring (1011) is rotatably sleeved inside the circular groove (602), and the circumferential surface of the sleeve ring (1011) is fixedly connected with the inner wall of the blanking pipe (101) through a plurality of fixing rods (1012).
5. The gas-solid method production process of cellulose mixed ether according to claim 2, 3 or 4, characterized in that:
the inner wall of the reaction kettle tank body (1) is provided with a toothed ring (5),
a plurality of auxiliary stirring devices (4) distributed in an annular array around the axis of the tank body (1) of the reaction kettle are arranged in the tank body,
the auxiliary stirring device (4) comprises a rotating shaft (401), a blade (402) and a first gear (403), one end of the rotating shaft (401) is inserted into the inner wall of the paddle shaft (3) or the paddle (301), the other end of the rotating shaft is fixedly connected with the first gear (403),
a plurality of blades (402) are fixedly connected with the circumferential surface of the rotating shaft (401),
the rotating shaft (401) is rotatably connected with the paddle shaft (3) or the paddle (301), the first gear (403) is arranged on the toothed ring (5), and the first gear (403) is meshed with the toothed ring (5).
6. The gas-solid method production process of cellulose mixed ether according to claim 5, characterized in that:
a driving mechanism is arranged above the upper cover (2) of the reaction kettle,
the driving mechanism comprises a first transmission rod (9), a second transmission rod (10), a third transmission rod (11), a fourth transmission rod (12), a fifth transmission rod (13) and a regulating device (14),
the first transmission rod (9) comprises a third bevel gear (901) and a first belt pulley (902) which are coaxially and fixedly connected through a rotating rod,
the second transmission rod (10) comprises a fourth bevel gear (1001), a second belt pulley (1002) and a third belt pulley (1003) which are coaxially and fixedly connected through a rotating rod,
the third transmission rod (11) comprises a driven gear (1101), a fourth belt pulley (1102), a second gear (1103) and a third gear (1104) which are coaxially and fixedly connected through a rotating rod,
the fourth transmission rod (12) comprises a fifth belt pulley (1201) and a fourth gear (1202) which are coaxially and fixedly connected through a rotating rod,
the fifth transmission rod (13) comprises a sixth belt pulley (1301) and a fifth gear (1302) which are coaxially and fixedly connected through a rotating rod,
the adjusting and controlling device (14) comprises a second telescopic rod (1401), a vertical rod (1402), an upper roller (1403) and a lower roller (1404) which are vertically arranged, the lower end of the vertical rod (1402) is fixedly connected with the top end of the telescopic part of the second telescopic rod (1401), the upper roller (1403) and the lower roller (1404) are respectively arranged at two sides of the vertical rod (1402) up and down, the axes of the upper roller (1403) and the lower roller (1404) are horizontally arranged,
the third bevel gear (901) is meshed with the second bevel gear (604), the first belt pulley (902) is connected with the fifth belt pulley (1201) through a first synchronous belt (15),
the fourth bevel gear (1001) is meshed with the first bevel gear (302), the second belt pulley (1002) is connected with the fourth belt pulley (1102) through a second synchronous belt (16), the third belt pulley (1003) is connected with the sixth belt pulley (1301) through a third synchronous belt (17),
the vertical rod (1402) is arranged between the second synchronous belt (16) and the third synchronous belt (17), the upper roller (1403) is positioned right above the second synchronous belt (16), the lower roller (1404) is positioned right below the third synchronous belt (17),
when the upper roller (1403) is not contacted with the second synchronous belt (16), the second synchronous belt (16) is in a loose state,
when the lower roller (1404) is not in contact with the third synchronous belt (17), the third synchronous belt (17) is in a relaxed state,
the driven gear (1101) is meshed with a driving gear (801) on an output shaft of the first motor (8), the second gear (1103) is meshed with the fifth gear (1302), and the third gear (1104) is meshed with the fourth gear (1202).
7. The gas-solid production process of cellulose mixed ether according to claim 1 or 6, characterized in that:
the separation device comprises three liquefaction tanks which are respectively used for liquefying ethylene oxide, chloromethane and dimethyl ether,
the liquefaction box comprises a first box body (19), the inner cavity of the first box body (19) is a cuboid, a snake-shaped refrigeration pipe (23) is arranged in the inner wall of the first box body (19) in the length direction, the inlet and the outlet of the snake-shaped refrigeration pipe (23) penetrate through the outer part of the first box body (19) and are communicated with the pipeline of the refrigeration unit,
an air inlet pipe (24) and an air outlet pipe (25) which are communicated with the inner cavity of the first box body (19) are arranged outside the first box body (19), a liquid discharge groove (1903) is concavely arranged at the bottom of the first box body (19), a liquid discharge pipe (27) is communicated and connected at the bottom of the liquid discharge groove (1903), the tail end of the liquid discharge pipe (27) is arranged outside the first box body (19) in a penetrating way,
a valve is arranged on the liquid discharge groove (1903) or the liquid discharge pipe (27),
an air inlet pipe (24) of a liquefaction box for liquefying the ethylene oxide is communicated with a pressure relief pipe (204) of the reaction kettle,
an exhaust pipe (25) of a liquefaction tank for liquefying ethylene oxide is communicated with an air inlet pipe (24) of a liquefaction tank for liquefying chloromethane,
an exhaust pipe (25) of a liquefied methane chloride tank is communicated with an air inlet pipe (24) of a liquefied dimethyl ether tank,
an exhaust pipe (25) of a liquefaction tank for liquefying dimethyl ether is communicated with the nitrogen recovery pipeline.
8. The gas-solid method production process of cellulose mixed ether according to claim 7, characterized in that:
a piston (20) is vertically arranged in the first box body (19), the peripheral end surfaces of the piston (20) are abutted against the inner wall of the first box body (19),
at least two screw rods (21) are arranged in the first box body (19) along the length direction, the screw rods (21) penetrate through the piston (20), the screw rods (21) are in threaded connection with the piston (20), one end of each screw rod (21) is inserted into the inner wall of the first box body (19), the other end of each screw rod (21) penetrates through the outer part of the first box body (19) and is fixedly connected with a seventh belt pulley (2101),
a second motor (22) is fixed to the outer portion of the first box body (19), an eighth belt pulley (2201) is fixed to an output shaft of the second motor (22), and the eighth belt pulley (2201) is connected with all the seventh belt pulleys (2101) through a same fourth synchronous belt (2202).
9. The gas-solid method production process of cellulose mixed ether according to claim 8, characterized in that:
the air inlet pipe (24) and the air outlet pipe (25) are connected with the side wall of one end of the first box body (19) in the length direction,
the side wall of the other end of the first box body (19) in the length direction is provided with a through hole (1902),
and a rubber sleeve (2001) is fixed at one end of the piston (20) facing the through hole (1902), and the rubber sleeve (2001) is in threaded connection with the screw (21).
10. The gas-solid method production process of cellulose mixed ether according to claim 9, characterized in that:
the outer part of the liquefaction box is provided with an air box (29), the air box (29) comprises a second box body (2901) with the upper end arranged in an open way,
an elastic gasket (2902) is arranged at the opening above the second box body (2901) in a covering way, the elastic gasket (2902) is fixedly connected with the second box body (2901) through a fixing frame (2903),
the outer part of the second box body (2901) is communicated with a test tube (2904), a stop valve is arranged on the test tube (2904),
the through hole (1902) is communicated with the second box body (2901) through a connecting air channel (30).
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310407104.3A CN116371333A (en) | 2022-03-29 | 2022-03-29 | Reaction kettle for producing cellulose mixed ether |
| CN202210324962.7A CN114713134A (en) | 2022-03-29 | 2022-03-29 | Gas-solid method for producing cellulose mixed ether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210324962.7A CN114713134A (en) | 2022-03-29 | 2022-03-29 | Gas-solid method for producing cellulose mixed ether |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310407104.3A Division CN116371333A (en) | 2022-03-29 | 2022-03-29 | Reaction kettle for producing cellulose mixed ether |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114713134A true CN114713134A (en) | 2022-07-08 |
Family
ID=82239975
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310407104.3A Pending CN116371333A (en) | 2022-03-29 | 2022-03-29 | Reaction kettle for producing cellulose mixed ether |
| CN202210324962.7A Pending CN114713134A (en) | 2022-03-29 | 2022-03-29 | Gas-solid method for producing cellulose mixed ether |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310407104.3A Pending CN116371333A (en) | 2022-03-29 | 2022-03-29 | Reaction kettle for producing cellulose mixed ether |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN116371333A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819629A (en) * | 2022-11-21 | 2023-03-21 | 重庆力宏精细化工有限公司 | High-temperature-resistant salt-resistant cellulose ether and preparation method and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3785430A (en) * | 1970-08-01 | 1974-01-15 | Huels Chemische Werke Ag | Cooling unit for large polymerization vessels |
| CN106939052A (en) * | 2017-03-24 | 2017-07-11 | 山东滕新材料股份有限公司 | A kind of preparation method of cellulose ether |
| CN110804103A (en) * | 2019-12-24 | 2020-02-18 | 山东赫达股份有限公司 | Gas-solid method production process of cellulose mixed ether |
| CN111214844A (en) * | 2020-01-17 | 2020-06-02 | 山东赫达股份有限公司 | Clean production system and process for cellulose mixed ether |
| CN111659334A (en) * | 2020-06-10 | 2020-09-15 | 合肥新坞岩机械科技有限公司 | Chemical reaction kettle |
| CN111886996A (en) * | 2020-08-20 | 2020-11-06 | 周鹏 | Depth-adjustable fertilizing system for agricultural machinery and using method |
| CN112629158A (en) * | 2020-12-25 | 2021-04-09 | 江苏国富氢能技术装备股份有限公司 | Hydrogen liquefaction system with ortho-para hydrogen conversion |
| CN213347834U (en) * | 2020-09-23 | 2021-06-04 | 临安市助剂化工有限公司 | Reaction kettle condensing device |
-
2022
- 2022-03-29 CN CN202310407104.3A patent/CN116371333A/en active Pending
- 2022-03-29 CN CN202210324962.7A patent/CN114713134A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3785430A (en) * | 1970-08-01 | 1974-01-15 | Huels Chemische Werke Ag | Cooling unit for large polymerization vessels |
| CN106939052A (en) * | 2017-03-24 | 2017-07-11 | 山东滕新材料股份有限公司 | A kind of preparation method of cellulose ether |
| CN110804103A (en) * | 2019-12-24 | 2020-02-18 | 山东赫达股份有限公司 | Gas-solid method production process of cellulose mixed ether |
| CN111214844A (en) * | 2020-01-17 | 2020-06-02 | 山东赫达股份有限公司 | Clean production system and process for cellulose mixed ether |
| CN111659334A (en) * | 2020-06-10 | 2020-09-15 | 合肥新坞岩机械科技有限公司 | Chemical reaction kettle |
| CN111886996A (en) * | 2020-08-20 | 2020-11-06 | 周鹏 | Depth-adjustable fertilizing system for agricultural machinery and using method |
| CN213347834U (en) * | 2020-09-23 | 2021-06-04 | 临安市助剂化工有限公司 | Reaction kettle condensing device |
| CN112629158A (en) * | 2020-12-25 | 2021-04-09 | 江苏国富氢能技术装备股份有限公司 | Hydrogen liquefaction system with ortho-para hydrogen conversion |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819629A (en) * | 2022-11-21 | 2023-03-21 | 重庆力宏精细化工有限公司 | High-temperature-resistant salt-resistant cellulose ether and preparation method and application thereof |
| CN115819629B (en) * | 2022-11-21 | 2024-01-30 | 重庆力宏精细化工有限公司 | High-temperature-resistant and salt-resistant cellulose ether and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116371333A (en) | 2023-07-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114713134A (en) | Gas-solid method for producing cellulose mixed ether | |
| CN110451756B (en) | Sequencing batch anaerobic digestion device based on thermal hydrolysis and membrane separation and use method thereof | |
| CN106673927A (en) | Cooling and conveying device | |
| CN115722154A (en) | Crotonic acid production system and technology | |
| CN113667540A (en) | Extraction device and extraction method of plant essential oil for cosmetic production | |
| CN112648536A (en) | Fluid infusion type oil-gas mixed transportation device | |
| CN112044380A (en) | Reaction system for polyurethane production | |
| CN111232979A (en) | Device for preparing super-capacitor activated carbon by alkali activation method and preparation method thereof | |
| CN111304948A (en) | High-pressure continuous horizontal pipe cooking pulping device | |
| CN205199501U (en) | Single cyandiamide exsolution system device of hydrolysising | |
| CN207996657U (en) | A kind of energy-saving and environment-friendly reaction kettle | |
| CN220931429U (en) | Small-sized fishing boat ice slurry preparation and purification integrated device | |
| CN203947087U (en) | For improving the equipment of coal slurry concentration | |
| CN219429939U (en) | Wet deslagging energy-saving system of coal gasification furnace | |
| CN218741828U (en) | Solvent driving and solvent recovery apparatus | |
| CN212090980U (en) | Freezing crystallization equipment for reducing salt concentration of chemical solution | |
| CN209679802U (en) | The device of hydrocarbon is mixed using liquid nitrogen recycling separation of olefins tail gas | |
| CN221076903U (en) | Cooling mechanism of compound apple juice | |
| CN215963155U (en) | Powder feeding device | |
| CN112212220B (en) | Liquid carbon dioxide supply and conveying system | |
| CN213088229U (en) | Single-screw air compressor for processing potato whole powder | |
| CN220657433U (en) | Acrylic resin high-pressure reaction kettle device | |
| CN219209940U (en) | Intelligent temperature control type mixing reaction kettle | |
| CN220507464U (en) | Vacuum drying device for preventing triethylene diamine from caking | |
| CN220091392U (en) | Hydrogenation reaction kettle |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220708 |