CN105694021A - Double-mode alkoxylation technique - Google Patents
Double-mode alkoxylation technique Download PDFInfo
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- CN105694021A CN105694021A CN201610193327.4A CN201610193327A CN105694021A CN 105694021 A CN105694021 A CN 105694021A CN 201610193327 A CN201610193327 A CN 201610193327A CN 105694021 A CN105694021 A CN 105694021A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/02—Preparation of ethers from oxiranes
- C07C41/03—Preparation of ethers from oxiranes by reaction of oxirane rings with hydroxy groups
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Abstract
The invention relates to a double-mode alkoxylation technique which is characterized by comprising the following steps: injecting a chain initiator into a vertical reactor; injecting an alkoxylating agent into the vertical reactor to carry out reaction; injecting an alkoxylating agent into a horizontal reactor to carry out reaction; injecting a liquid phase and a gas phase into a gas-liquid mixer; carrying out reaction control; carrying out reaction curing; and treating the reaction residual gas. The technique achieves the goal of double-mode alkoxylation reaction, and the operation process is automatically controlled by a programming controller, thereby ensuring the whole technical process to operate safely and stably. The feed rate of the alkoxylating agent (epoxyethane or epoxypropane) can reach 30 tons/hour, and the reaction period for each batch can be shortened to 2/3 of that of the single-mode reactor. The efficiency is enhanced by at least 30% as compared with the single-mode reactor, and is 5-7 times of that of the traditional reactor.
Description
Technical field
The invention belongs to petrochemical industry, more particularly, it relates to a kind of double mode alkoxylation process based on aerosol+gas-liquid, for ethoxylation, propoxylation reaction。
Background technology
Current domestic and international application mainly stirs autoclave alkoxylation production technology, Italy's Press company atomizing alkoxylation production technology and Buss company of Switzerland loop-jet alkoxylation production technology exactly in the reaction production technology of alkoxylate (second/propoxylation) production field。Stirring autoclave alkoxylation production technology belongs to gas liquid reaction, and heat exchange efficiency is low；Press company of Italy atomizing alkoxylation production technology belongs to gas-droplet (hereinafter referred to as " aerosol ") reaction, although heat exchange efficiency is high, and response speed is higher, but response speed is still restricted；Buss company of Switzerland loop-jet alkoxylation production technology belongs to bubble-liquid (hereinafter referred to as " gas-liquid ") reaction, and heat exchange efficiency, response speed are also higher, but still not ideal enough。
Summary of the invention
The present invention seeks to: overcome the deficiencies in the prior art, it is provided that a kind of double mode alkoxylation process of aerosol+gas-liquid。
This invention address that the scheme of technical problem is: a kind of double mode alkoxylation process, it is characterized in that: comprise the following steps:
1) start of chain agent is injected to vertical reactor
1. by cyclelog control, start of chain agent feeding line injects start of chain agent by the start of chain agent import of vertical reactor, and liquid level detector monitors the liquid level in vertical reactor in real time, stops charging when liquid level reaches the first setting value；
2. while injecting start of chain agent, by cyclelog control, by catalyst feed line to vertical reactor injecting catalyst, when reaching set amount, injecting catalyst is stopped；
3. by cyclelog control, start partial circulating pump, start of chain agent in vertical reactor is exported by the partial circulating of vertical reactor bottom surface and enters partial circulating loop, flows successively through partial circulating pump and partial circulating heat exchanger, the partial circulating entrance on vertical reactor top flows back to vertical reactor；
4. while start of chain agent enters partial circulating loop, by cyclelog control, start the heating circuit of partial circulating heat exchanger, the start of chain agent flowing through partial circulating heat exchanger is heated to design temperature；
5., before start of chain agent is reacted with oxyalkylated reagent, process unit nitrogen used is replaced, and makes oxygen content in process unit reach below 80ppm；
2) inject oxyalkylated reagent to vertical reactor to react
1. after start of chain agent temperature reaches setting value, by cyclelog control, opening the first charging internally piloted valve, close charging internally piloted valve, the oxyalkylated reagent entrance that oxyalkylated reagent feeding line is arranged by vertical reactor end face injects oxyalkylated reagent, starts to react in vertical reactor；
2. while starting in vertical reactor to react, by cyclelog control, start the cooling circuit of partial circulating heat exchanger, the material flowing through partial circulating heat exchanger is cooled down；
3) inject oxyalkylated reagent to horizontal reactor to react
1. in vertical reactor, liquid level reaches the second setting value, by cyclelog control, open systemic circulation internally piloted valve, close liquid phase internally piloted valve, start systemic circulation pump, material in vertical reactor is exported by the systemic circulation of vertical reactor bottom and enters systemic circulation loop, flow successively through systemic circulation pump, systemic circulation heat exchanger and systemic circulation internally piloted valve, the systemic circulation entrance of horizontal reactor side flow in horizontal reactor；
2. while the material in systemic circulation loop enters horizontal reactor, by cyclelog control, open the second charging internally piloted valve, oxyalkylated reagent feeding line inject oxyalkylated reagent by some oxyalkylated reagent imports of horizontal reactor end face, start in horizontal reactor to react；
3. while starting in horizontal reactor to react, by cyclelog control, start the cooling circuit of systemic circulation heat exchanger, the material flowing through systemic circulation heat exchanger is cooled down；
4) liquid and gas are injected to air and liquid mixer
In vertical reactor, liquid level reaches the 3rd setting value, by cyclelog control, open the liquid phase internally piloted valve before air and liquid mixer and gas phase internally piloted valve simultaneously, the material of systemic circulation heat exchanger is flowed out by the liquid phase internally piloted valve before air and liquid mixer by systemic circulation heat exchanger exit, air and liquid mixer is entered by the liquid phase entrance of air and liquid mixer, the gas phase flowed out by vertical reactor end face gaseous phase outlet is by the gas phase internally piloted valve before air and liquid mixer, air and liquid mixer is entered by the gas phase entrance of air and liquid mixer, now, gas phase and liquid phase react simultaneously in air and liquid mixer and vertical reactor simultaneously；
5) reaction controlling
Reaction temperature controls at 100～190 DEG C, and reaction pressure controls at 0.3～0.6Mpa, and oxyalkylated reagent charging rate reaches 30 ton hour；
6) reaction ripening
After oxyalkylated reagent injection rate reaches setting value, by cyclelog control, close the first charging internally piloted valve and the second charging internally piloted valve of oxyalkylated reagent feeding line, keep partial circulating loop and systemic circulation loop unimpeded, keep Matter Transfer and control reaction temperature and carry out ripening, until completing ripening；
7) reaction residual gas processes。
The structure of described double mode alkoxylation technique equipment therefor is: it includes vertical reactor, horizontal reactor, partial circulating pump, partial circulating heat exchanger, systemic circulation pump, systemic circulation heat exchanger and cyclelog, the end face of described vertical reactor is respectively provided with oxyalkylated reagent entrance, series connection entrance and gaseous phase outlet, bottom surface arranges partial circulating outlet, the top of vertical reactor arranges partial circulating entrance, bottom arranges systemic circulation outlet, the centre of vertical reactor arranges start of chain agent import and gas-liquid is mixed into mouth, the oxyalkylated reagent entrance of vertical reactor is connected with oxyalkylated reagent feeding line by the first charging internally piloted valve, start of chain agent import is connected with start of chain agent feeding line, temperature detector and liquid level detector are set in the bottom of vertical reactor；Described horizontal reactor be arranged above with some oxyalkylated reagent imports, the side of horizontal reactor arranges systemic circulation entrance, bottom surface arranges series connection outlet, the oxyalkylated reagent import of horizontal reactor is connected with oxyalkylated reagent feeding line by the second charging internally piloted valve, the entrance of connecting that the series connection outlet that horizontal reactor is arranged by bottom surface is arranged with vertical reactor top connects, between partial circulating outlet and the partial circulating entrance of vertical reactor top setting that vertical reactor bottom surface is arranged, it is sequentially connected with partial circulating pump and partial circulating heat exchanger constitutes partial circulating loop, between the partial circulating heat exchanger and the partial circulating entrance of vertical reactor in partial circulating loop, catalyst feed line is set；Between systemic circulation outlet and the systemic circulation entrance of horizontal reactor side setting that vertical reactor bottom is arranged, it is sequentially connected with systemic circulation pump, systemic circulation heat exchanger and systemic circulation internally piloted valve constitutes systemic circulation loop, the gas phase entrance of air and liquid mixer is connected with gas phase internally piloted valve and passes through gas phase internally piloted valve and is connected with the gaseous phase outlet of vertical reactor end face, the liquid phase entrance of air and liquid mixer is connected with liquid phase internally piloted valve and passes through liquid phase internally piloted valve and is connected with the outlet of systemic circulation heat exchanger, and the gas liquid outlet of air and liquid mixer is connected with the gas-liquid entrance of vertical reactor；Described temperature detector, liquid level detector, the first charging internally piloted valve, the second charging internally piloted valve, systemic circulation internally piloted valve, gas phase internally piloted valve and liquid phase internally piloted valve are connected with cyclelog signal respectively。
The invention has the beneficial effects as follows:
1 present invention is to carry out in horizontal reactor carrying out aerosol-gas liquid reaction in aerosol reaction, vertical reactor and realizing gas liquid reaction by an air and liquid mixer simultaneously, achieve and double mode complete the target that alkoxylate is anti-, running is automatically controlled by cyclelog, it is ensured that whole technical process safe and stable operation；Oxygen base agent (oxirane or expoxy propane) charging rate can reach 30 ton hour, and every batch of reaction time can foreshorten to the 2/3 of monotype reactor。At least improve the efficiency of 30% than monotype reactor, be the efficiency of 5～7 times of traditional reactor。
The instantaneous storage of oxyalkylated reagent in 2 vertical reactors and horizontal reactor, well below the reactor of prior art；In course of reaction, in liquid phase, unreacted and insoluble alkoxylate agent concentration are very low；High reaction rate makes the oxyalkylated reagent of vaporization convert continuously, it is to avoid the generation of autohemagglutination；
3 replace stirring-type reactor with double mode reactor, it does not have the rotary type parts of stirrer contact with gas phase；It is prevented from liquid and can not flow back to oxyalkylated reagent alkane basin；In gas-to-liquid contact, owing to gas phase has higher conductivity, in reactor, there is no the generation of electric spark；Large and small circulation instead of stirring, it is ensured that mixing of materials is more abundant, reacts more complete；
The cooling system of 4 equipment therefors of the present invention can take away epoxy second/propane feed speed maximum time produce heat, reactor, by low-pressure steam, can make production temperature exceed minimum permissible temperature。
Accompanying drawing explanation
Accompanying drawing 1 is the double mode alkoxylation process process schematic of one of the present invention。
1 vertical reactor in figure, 2 horizontal reactors, 3 air and liquid mixers, 4 systemic circulation heat exchangers, 5 partial circulating heat exchangers, 6 systemic circulation pumps, 7 partial circulating pumps, 8 oxyalkylated reagent feeding lines, 9 start of chain agent feeding lines, 10 first charging internally piloted valves, 11 second charging internally piloted valves, 12 gas phase internally piloted valves, 13 liquid phase internally piloted valves, 14 systemic circulation internally piloted valves, 15 cyclelogs, 16 catalyst feed line。
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is further described。
Referring to Fig. 1, embodiment 1 the present embodiment is to produce C(12-14)AEO3For example。
1) start of chain agent is injected to vertical reactor 1
1. being controlled by cyclelog 15, start of chain agent feeding line 9 injects start of chain agent C12-14 alcohol by the start of chain agent import of vertical reactor 1, and injection rate reaches 7320 kilograms and stops charging；
2. while injecting start of chain agent, cyclelog 15 controlling, by catalyst feed line 16 to vertical reactor 1 injecting catalyst KOH, injection rate stops injecting catalyst when reaching 36 kilograms；
3. controlled by cyclelog 15, start partial circulating pump 7, entrance partial circulating loop is exported by the start of chain agent of catalysis by the partial circulating of vertical reactor 1 bottom surface in vertical reactor 1, flow successively through partial circulating pump 7 and partial circulating heat exchanger 5, the partial circulating entrance on vertical reactor 1 top flow back to vertical reactor 1；
4. while start of chain agent enters partial circulating loop, cyclelog 15 control, start the heating circuit of partial circulating heat exchanger 5, the start of chain agent flowing through partial circulating heat exchanger 5 is heated to reacting initial temperature 120-160 DEG C；
5., before start of chain agent with reacting ethylene oxide, process unit nitrogen used is replaced, and makes oxygen content in process unit reach below 80ppm；
2) react to vertical reactor 1 injection ring oxidative ethane
1. after start of chain agent temperature reaches 120-160 DEG C, controlled by cyclelog 15, open the first charging internally piloted valve 10, close the second charging internally piloted valve 11, the oxyalkylated reagent entrance that oxyalkylated reagent feeding line 8 is arranged by vertical reactor 1 end face injects alkane oxirane, starts to react in vertical reactor 1；
2. while starting to react in vertical reactor 1, controlled by cyclelog 15, start the cooling circuit of partial circulating heat exchanger 5, the reaction heat conduction oil flowing through the material of partial circulating heat exchanger 5 is removed, thus the material flowing through partial circulating heat exchanger 5 is cooled down；
3) react to horizontal reactor 2 injection ring oxidative ethane
1. in vertical reactor 1, liquid level reaches the second setting value, controlled by cyclelog 15, open systemic circulation internally piloted valve 14, close liquid phase internally piloted valve 13, start systemic circulation pump 6, material in vertical reactor 1 is exported by the systemic circulation of vertical reactor 1 bottom and enters systemic circulation loop, flow successively through systemic circulation pump 6, systemic circulation heat exchanger 4 and systemic circulation internally piloted valve 14, the systemic circulation entrance of horizontal reactor 2 side flow in horizontal reactor 2；
2. while the material in systemic circulation loop enters horizontal reactor 2, controlled by cyclelog 15, open the second charging internally piloted valve 11, passed through some oxyalkylated reagent import injection ring oxidative ethanes of horizontal reactor 2 end face by oxyalkylated reagent feeding line 8, start to react in horizontal reactor 2；
3. while starting to react in horizontal reactor 2, controlled by cyclelog 15, start the cooling circuit of systemic circulation heat exchanger 4, the reaction heat conduction oil flowing through the material of systemic circulation heat exchanger 4 is removed, thus the material flowing through systemic circulation heat exchanger 4 is cooled down；
4) liquid and gas are injected to air and liquid mixer 3
In vertical reactor 1, liquid level reaches the 3rd setting value, controlled by cyclelog 15, open the liquid phase internally piloted valve 13 before air and liquid mixer 3 and gas phase internally piloted valve 12 simultaneously, the material flowing out systemic circulation heat exchanger 4 is exported by the liquid phase internally piloted valve 13 before air and liquid mixer 3 by systemic circulation heat exchanger 4, air and liquid mixer 3 is entered by the liquid phase entrance of air and liquid mixer 3, the gas phase flowed out by vertical reactor 1 end face gaseous phase outlet is by the gas phase internally piloted valve 12 before air and liquid mixer 3, air and liquid mixer 3 is entered by the gas phase entrance of air and liquid mixer 3, now, gas phase and liquid phase react simultaneously in air and liquid mixer 3 and vertical reactor 1 simultaneously；
5) reaction controlling
Reaction temperature controls at 100～190 DEG C, and reaction pressure controls at 0.3～0.6Mpa；
6) reaction ripening
After oxirane injection rate reaches 4812 kilograms of setting, controlled by cyclelog 15, close the first charging internally piloted valve 10 and the second charging internally piloted valve 11 of oxyalkylated reagent feeding line 8, now, a small amount of oxirane is still had to be present in gas phase and be dissolved in liquid phase, therefore keep partial circulating loop and systemic circulation loop unimpeded, keep Matter Transfer and control reaction temperature and carry out ripening, until completing ripening, < 0.1MPa when the residual pressure of vertical reactor 1 is constant, namely thinks that reaction terminates；
7) reaction residual gas processes
After reaction terminates, first residual gas in process unit used is drained into exhaust gas treatment unit, then degassed under vacuo, and keep reactant to circulate, until product circulating cooling to 50-110 DEG C, with the arbitrary of systemic circulation pump 6 and partial circulating pump 7 or be discharged in neutralizer by product simultaneously, in process unit used, remaining product nitrogen blows out。Every batch can produce C (12-14) AEO312 ton。
The present embodiment ethylene oxide feed rate can reach 30 ton hour, and every batch of reaction time can foreshorten to the 2/3 of monotype reactor。At least improve the efficiency of 30% than monotype reactor, be the efficiency of 5～7 times of traditional reactor。
The structure of process unit used by the present embodiment is: it includes vertical reactor 1, horizontal reactor 2, partial circulating pump 7, partial circulating heat exchanger 5, systemic circulation pump 6, systemic circulation heat exchanger 4 and cyclelog 15, the end face of described vertical reactor 1 is respectively provided with oxyalkylated reagent entrance, series connection entrance and gaseous phase outlet, bottom surface arranges partial circulating outlet, the top of vertical reactor 1 arranges partial circulating entrance, bottom arranges systemic circulation outlet, the centre of vertical reactor 1 arranges start of chain agent import and gas-liquid is mixed into mouth, the oxyalkylated reagent entrance of vertical reactor 1 is connected with oxyalkylated reagent feeding line 8 by the first charging internally piloted valve 10, start of chain agent import is connected with start of chain agent feeding line 9, temperature detector and liquid level detector are set in the bottom of vertical reactor 1；Described horizontal reactor 2 be arranged above with some oxyalkylated reagent imports, the side of horizontal reactor 2 arranges systemic circulation entrance, bottom surface arranges series connection outlet, the oxyalkylated reagent import of horizontal reactor 2 is connected with oxyalkylated reagent feeding line 8 by the second charging internally piloted valve 11, the entrance of connecting that the series connection outlet that horizontal reactor 2 is arranged by bottom surface is arranged with vertical reactor 1 top connects, between partial circulating outlet and the partial circulating entrance of vertical reactor 1 top setting that vertical reactor 1 bottom surface is arranged, it is sequentially connected with partial circulating pump 7 and partial circulating heat exchanger 5 constitutes partial circulating loop, between the partial circulating heat exchanger 5 and the partial circulating entrance of vertical reactor 1 in partial circulating loop, catalyst feed line 16 is set；It is sequentially connected with systemic circulation pump 6 between systemic circulation outlet and the systemic circulation entrance of horizontal reactor 2 side setting that vertical reactor 1 bottom is arranged, systemic circulation heat exchanger 4 and systemic circulation internally piloted valve 14 constitute systemic circulation loop, the gas phase entrance of air and liquid mixer 3 is connected with gas phase internally piloted valve 12, and be connected with the gaseous phase outlet of vertical reactor 1 end face by gas phase internally piloted valve 12, the liquid phase entrance of air and liquid mixer 3 is connected with liquid phase internally piloted valve 13, and be connected with the outlet of systemic circulation heat exchanger 4 by liquid phase internally piloted valve 13, the gas liquid outlet of air and liquid mixer 3 is connected with the gas-liquid entrance of vertical reactor 1；Described temperature detector, liquid level detector, first charging internally piloted valve the 10, second charging internally piloted valve 11, systemic circulation internally piloted valve 14, gas phase internally piloted valve 12 and liquid phase internally piloted valve 13 are connected with cyclelog 15 signal respectively。
Process unit used by the present embodiment adopts prior art manufacture, and described temperature detector, liquid level detector, first charging internally piloted valve the 10, second charging internally piloted valve 11, systemic circulation internally piloted valve 14, gas phase internally piloted valve 12, liquid phase internally piloted valve 13 and cyclelog 15 are the commercially available prod of prior art。
Embodiment 2, the present embodiment is to produce HPEG
One, HPEG400 intermediate synthesis
1) start of chain agent is injected to vertical reactor 1
1. being controlled by cyclelog 15, start of chain agent feeding line 9 injects start of chain agent methallyl alcohol by the start of chain agent import of vertical reactor 1, and injection rate reaches 840 kilograms and stops charging；
2. while injecting start of chain agent, cyclelog 15 controlling, by catalyst feed line 16 to vertical reactor 1 injecting catalyst, injection rate stops injecting catalyst when reaching setting value；
3. controlled by cyclelog 15, start partial circulating pump 7, entrance partial circulating loop is exported by the start of chain agent of catalysis by the partial circulating of vertical reactor 1 bottom surface in vertical reactor 1, flow successively through partial circulating pump 7 and partial circulating heat exchanger 5, the partial circulating entrance on vertical reactor 1 top flow back to vertical reactor 1；
4. while start of chain agent enters partial circulating loop, cyclelog 15 control, start the heating circuit of partial circulating heat exchanger 5, the start of chain agent flowing through partial circulating heat exchanger 5 is heated to reacting initial temperature 100 DEG C；
5., before start of chain agent with reacting ethylene oxide, process unit nitrogen used is replaced, and makes oxygen content in process unit reach below 80ppm；
2) inject oxyalkylated reagent to vertical reactor 1 to react
1. after start of chain agent temperature reaches 100 DEG C, controlled by cyclelog 15, open the first charging internally piloted valve 10, close the second charging internally piloted valve 11, the oxyalkylated reagent entrance injection ring oxidative ethane that oxyalkylated reagent feeding line 8 is arranged by vertical reactor 1 end face, starts to react in vertical reactor 1；
2. while starting to react in vertical reactor 1, controlled by cyclelog 15, start the cooling circuit of partial circulating heat exchanger 5, the reaction heat conduction oil flowing through the material of partial circulating heat exchanger 5 is removed, thus the material flowing through partial circulating heat exchanger 5 is cooled down；
3) react to horizontal reactor 2 injection ring oxidative ethane
1. in vertical reactor 1, liquid level reaches the second setting value, controlled by cyclelog 15, open systemic circulation internally piloted valve 14, close liquid phase internally piloted valve 13, start systemic circulation pump 6, material in vertical reactor 1 is exported by the systemic circulation of vertical reactor 1 bottom and enters systemic circulation loop, flow successively through systemic circulation pump 6, systemic circulation heat exchanger 4 and systemic circulation internally piloted valve 14, the systemic circulation entrance of horizontal reactor 2 side flow in horizontal reactor 2；
2. while the material in systemic circulation loop enters horizontal reactor 2, controlled by cyclelog 15, open the second charging internally piloted valve 11, passed through some oxyalkylated reagent import injection ring oxidative ethanes of horizontal reactor 2 end face by oxyalkylated reagent feeding line 8, start to react in horizontal reactor 2；
3. while starting to react in horizontal reactor 2, controlled by cyclelog 15, start the cooling circuit of systemic circulation heat exchanger 4, the reaction heat conduction oil flowing through the material of systemic circulation heat exchanger 4 is removed, thus the material flowing through systemic circulation heat exchanger 4 is cooled down；
4) liquid and gas are injected to air and liquid mixer 3
In vertical reactor 1, liquid level reaches the 3rd setting value, controlled by cyclelog 15, open the liquid phase internally piloted valve 13 before air and liquid mixer 3 and gas phase internally piloted valve 12 simultaneously, the material flowing out systemic circulation heat exchanger 4 is exported by the liquid phase internally piloted valve 13 before air and liquid mixer 3 by systemic circulation heat exchanger 4, air and liquid mixer 3 is entered by the liquid phase entrance of air and liquid mixer 3, the gas phase flowed out by vertical reactor 1 end face gaseous phase outlet is by the gas phase internally piloted valve 12 before air and liquid mixer 3, air and liquid mixer 3 is entered by the gas phase entrance of air and liquid mixer 3, now, gas phase and liquid phase react simultaneously in air and liquid mixer 3 and vertical reactor 1 simultaneously；
5) reaction controlling
Reaction temperature controls on 100～110 DEG C of top, 125～130 DEG C, bottom, and reaction pressure controls at 0.38MPa；
6) reaction ripening
After oxirane injection rate reaches 3860 kilograms of setting, controlled by cyclelog 15, close the first charging internally piloted valve 10 and the second charging internally piloted valve 11 of oxyalkylated reagent feeding line 8, now, a small amount of oxirane is still had to be present in gas phase and be dissolved in liquid phase, therefore keep partial circulating loop and systemic circulation loop unimpeded, keep Matter Transfer and control reaction temperature and carry out ripening, until completing ripening, < 0.1MPa when the residual pressure of vertical reactor 1 is constant, namely thinks that reaction terminates；
7) reaction residual gas processes
After reaction terminates, first residual gas in process unit used is drained into exhaust gas treatment unit, then degassed under vacuo, and keep reactant to circulate, until product circulating cooling to 50-110 DEG C, with the arbitrary of systemic circulation pump 6 and partial circulating pump or be discharged in neutralizer by product simultaneously, using remaining product nitrogen blowout in process unit, intermediate storage tank sent into by material；
Two, HPEG2400 finished product synthesis
1) start of chain agent is injected to vertical reactor 1
1. being controlled by cyclelog 15, start of chain agent feeding line 9 injects start of chain agent HPEG400 by the start of chain agent import of vertical reactor 1, and injection rate reaches 2350 kilograms and stops charging；
2. controlled by cyclelog 15, start partial circulating pump 7, entrance partial circulating loop is exported by the start of chain agent of catalysis by the partial circulating of vertical reactor 1 bottom surface in vertical reactor 1, flow successively through partial circulating pump 7 and partial circulating heat exchanger 5, the partial circulating entrance on vertical reactor 1 top flow back to vertical reactor 1；
3. while start of chain agent enters partial circulating loop, cyclelog 15 control, start the heating circuit of partial circulating heat exchanger 5, the start of chain agent flowing through partial circulating heat exchanger 5 is heated to reacting initial temperature 100 DEG C；
4., before start of chain agent with reacting ethylene oxide, process unit nitrogen used is replaced, and makes oxygen content in process unit reach below 80ppm；
2) react to vertical reactor 1 injection ring oxidative ethane
1. after start of chain agent temperature reaches 100 DEG C, controlled by cyclelog 15, open the first charging internally piloted valve 10, close the second charging internally piloted valve 11, the oxyalkylated reagent entrance injection ring oxidative ethane that oxyalkylated reagent feeding line 8 is arranged by vertical reactor 1 end face, starts to react in vertical reactor 1；
2. while starting to react in vertical reactor 1, controlled by cyclelog 15, start the cooling circuit of partial circulating heat exchanger 5, the reaction heat conduction oil flowing through the material of partial circulating heat exchanger 5 is removed, thus the material flowing through partial circulating heat exchanger 5 is cooled down；
3) react to horizontal reactor 2 injection ring oxidative ethane
1. in vertical reactor 1, liquid level reaches the second setting value, controlled by cyclelog 15, open systemic circulation internally piloted valve 14, close liquid phase internally piloted valve 13, start systemic circulation pump 6, material in vertical reactor 1 is exported by the systemic circulation of vertical reactor 1 bottom and enters systemic circulation loop, flow successively through systemic circulation pump 6, systemic circulation heat exchanger 4 and systemic circulation internally piloted valve 14, the systemic circulation entrance of horizontal reactor 2 side flow in horizontal reactor 2；
2. while the material in systemic circulation loop enters horizontal reactor 2, controlled by cyclelog 15, open the second charging internally piloted valve 11, passed through some oxyalkylated reagent import injection ring oxidative ethanes of horizontal reactor 2 end face by oxyalkylated reagent feeding line 8, start to react in horizontal reactor 2；
3. while starting to react in horizontal reactor 2, controlled by cyclelog 15, start the cooling circuit of systemic circulation heat exchanger 4, the reaction heat conduction oil flowing through the material of systemic circulation heat exchanger 4 is removed, thus the material flowing through systemic circulation heat exchanger 4 is cooled down；
4) liquid and gas are injected to air and liquid mixer 3
In vertical reactor 1, liquid level reaches the 3rd setting value, controlled by cyclelog 15, open the liquid phase internally piloted valve 13 before air and liquid mixer 3 and gas phase internally piloted valve 12 simultaneously, the material flowing out systemic circulation heat exchanger 4 is exported by the liquid phase internally piloted valve 13 before air and liquid mixer 3 by systemic circulation heat exchanger 4, air and liquid mixer 3 is entered by the liquid phase entrance of air and liquid mixer 3, the gas phase flowed out by vertical reactor 1 end face gaseous phase outlet is by the gas phase internally piloted valve 12 before air and liquid mixer 3, air and liquid mixer 3 is entered by the gas phase entrance of air and liquid mixer 3, now, gas phase and liquid phase react simultaneously in air and liquid mixer 3 and vertical reactor 1 simultaneously；
5) reaction controlling
Reaction temperature controls on 100～110 DEG C of top, 125～130 DEG C, bottom, and reaction pressure controls at 0.38MPa；
6) reaction ripening
After oxyalkylated reagent injection rate reaches 11650 kilograms of setting, controlled by cyclelog 15, close the first charging internally piloted valve 10 and the second charging internally piloted valve 11 of oxyalkylated reagent feeding line 8, now, a small amount of oxirane is still had to be present in gas phase and be dissolved in liquid phase, therefore keep partial circulating loop and systemic circulation loop unimpeded, keep Matter Transfer and control reaction temperature and carry out ripening, until completing ripening, < 0.1MPa when the residual pressure of vertical reactor 1 is constant, namely thinks that reaction terminates；
7) reaction residual gas processes
After reaction terminates, first residual gas in process unit used is drained into exhaust gas treatment unit, then degassed under vacuo, and keep reactant to circulate, until product circulating cooling to 90 DEG C, with the arbitrary of systemic circulation pump 6 and partial circulating pump or be discharged in neutralizer by product simultaneously, the remaining product nitrogen of process unit is used to blow out, storage tank sent into by material, and every batch can produce 14 tons of HPEG2400。
Process unit used by the present embodiment is identical with embodiment 1。
Claims (2)
1. a double mode alkoxylation process, is characterized in that: comprise the following steps:
1) start of chain agent is injected to vertical reactor
1. by cyclelog control, start of chain agent feeding line injects start of chain agent by the start of chain agent import of vertical reactor, and liquid level detector monitors the liquid level in vertical reactor in real time, stops charging when liquid level reaches the first setting value；
2. while injecting start of chain agent, by cyclelog control, by catalyst feed line to vertical reactor injecting catalyst, when reaching set amount, injecting catalyst is stopped；
3. by cyclelog control, start partial circulating pump, start of chain agent in vertical reactor is exported by the partial circulating of vertical reactor bottom surface and enters partial circulating loop, flows successively through partial circulating pump and partial circulating heat exchanger, the partial circulating entrance on vertical reactor top flows back to vertical reactor；
4. while start of chain agent enters partial circulating loop, by cyclelog control, start the heating circuit of partial circulating heat exchanger, the start of chain agent flowing through partial circulating heat exchanger is heated to design temperature；
5., before start of chain agent is reacted with oxyalkylated reagent, process unit nitrogen used is replaced, and makes oxygen content in process unit reach below 80ppm；
2) inject oxyalkylated reagent to vertical reactor to react
1. after start of chain agent temperature reaches setting value, by cyclelog control, opening the first charging internally piloted valve, close the second charging control valve, the oxyalkylated reagent entrance that oxyalkylated reagent feeding line is arranged by vertical reactor end face injects oxyalkylated reagent, starts to react in vertical reactor；
2. while starting in vertical reactor to react, by cyclelog control, start the cooling circuit of partial circulating heat exchanger, the material flowing through partial circulating heat exchanger is cooled down；
3) inject oxyalkylated reagent to horizontal reactor to react
1. in vertical reactor, liquid level reaches the second setting value, by cyclelog control, open systemic circulation internally piloted valve, close liquid phase internally piloted valve, start systemic circulation pump, material in vertical reactor is exported by the systemic circulation of vertical reactor bottom and enters systemic circulation loop, flow successively through systemic circulation pump, systemic circulation heat exchanger and systemic circulation internally piloted valve, the systemic circulation entrance of horizontal reactor side flow in horizontal reactor；
2. while the material in systemic circulation loop enters horizontal reactor, by cyclelog control, open the second charging internally piloted valve, oxyalkylated reagent feeding line inject oxyalkylated reagent by some oxyalkylated reagent imports of horizontal reactor end face, start in horizontal reactor to react；
3. while starting in horizontal reactor to react, by cyclelog control, start the cooling circuit of systemic circulation heat exchanger, the material flowing through systemic circulation heat exchanger is cooled down；
4) liquid and gas are injected to air and liquid mixer
In vertical reactor, liquid level reaches the 3rd setting value, by cyclelog control, open the liquid phase internally piloted valve before air and liquid mixer and gas phase internally piloted valve simultaneously, the material of systemic circulation heat exchanger is flowed out by the liquid phase internally piloted valve before air and liquid mixer by systemic circulation heat exchanger exit, air and liquid mixer is entered by the liquid phase entrance of air and liquid mixer, the gas phase flowed out by vertical reactor end face gaseous phase outlet is by the gas phase internally piloted valve before air and liquid mixer, air and liquid mixer is entered by the gas phase entrance of air and liquid mixer, now, gas phase and liquid phase react simultaneously in air and liquid mixer and vertical reactor simultaneously；
5) reaction temperature controls at 100～190 DEG C, and reaction pressure controls at 0.3～0.6Mpa, and oxyalkylated reagent charging rate reaches 30 ton hour；
6) reaction ripening
After oxyalkylated reagent injection rate reaches setting value, by cyclelog control, close the first charging internally piloted valve and the second charging internally piloted valve of oxyalkylated reagent feeding line, keep partial circulating loop and systemic circulation loop unimpeded, keep Matter Transfer and control reaction temperature and carry out ripening, until completing ripening；
7) reaction residual gas processes。
2. a kind of double mode alkoxylation process as claimed in claim 1, it is characterized in that: described step 2) structure of equipment therefor is: it includes vertical reactor, horizontal reactor, partial circulating pump, partial circulating heat exchanger, systemic circulation pump, systemic circulation heat exchanger and cyclelog, the end face of described vertical reactor is respectively provided with oxyalkylated reagent entrance, series connection entrance and gaseous phase outlet, bottom surface arranges partial circulating outlet, the top of vertical reactor arranges partial circulating entrance, bottom arranges systemic circulation outlet, the centre of vertical reactor arranges start of chain agent import and gas-liquid is mixed into mouth, the oxyalkylated reagent entrance of vertical reactor is connected with oxyalkylated reagent feeding line by the first charging internally piloted valve, start of chain agent import is connected with start of chain agent feeding line, temperature detector and liquid level detector are set in the bottom of vertical reactor；Described horizontal reactor be arranged above with some oxyalkylated reagent imports, the side of horizontal reactor arranges systemic circulation entrance, bottom surface arranges series connection outlet, the oxyalkylated reagent import of horizontal reactor is connected with oxyalkylated reagent feeding line by the second charging internally piloted valve, the entrance of connecting that the series connection outlet that horizontal reactor is arranged by bottom surface is arranged with vertical reactor top connects, between partial circulating outlet and the partial circulating entrance of vertical reactor top setting that vertical reactor bottom surface is arranged, it is sequentially connected with partial circulating pump and partial circulating heat exchanger constitutes partial circulating loop, between the partial circulating heat exchanger and the partial circulating entrance of vertical reactor in partial circulating loop, catalyst feed line is set；Between systemic circulation outlet and the systemic circulation entrance of horizontal reactor side setting that vertical reactor bottom is arranged, it is sequentially connected with systemic circulation pump, systemic circulation heat exchanger and systemic circulation internally piloted valve constitutes systemic circulation loop, the gas phase entrance of air and liquid mixer is connected with gas phase internally piloted valve and passes through gas phase internally piloted valve and is connected with the gaseous phase outlet of vertical reactor end face, the liquid phase entrance of air and liquid mixer is connected with liquid phase internally piloted valve and passes through liquid phase internally piloted valve and is connected with the outlet of systemic circulation heat exchanger, and the gas liquid outlet of air and liquid mixer is connected with the gas-liquid entrance of vertical reactor；Described temperature detector, liquid level detector, the first charging internally piloted valve, the second charging internally piloted valve, systemic circulation internally piloted valve, gas phase internally piloted valve and liquid phase internally piloted valve are connected with cyclelog signal respectively。
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