CN110180463A - A kind of system and method automatically controlling autoclave heating cooling - Google Patents
A kind of system and method automatically controlling autoclave heating cooling Download PDFInfo
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- CN110180463A CN110180463A CN201910385593.0A CN201910385593A CN110180463A CN 110180463 A CN110180463 A CN 110180463A CN 201910385593 A CN201910385593 A CN 201910385593A CN 110180463 A CN110180463 A CN 110180463A
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 65
- 238000001816 cooling Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 186
- 230000001105 regulatory effect Effects 0.000 claims abstract description 104
- 238000004321 preservation Methods 0.000 claims abstract description 25
- 239000000498 cooling water Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 230000001276 controlling effect Effects 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 claims 1
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 5
- 238000012546 transfer Methods 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 230000006641 stabilisation Effects 0.000 abstract description 3
- 238000011105 stabilization Methods 0.000 abstract description 3
- 238000009834 vaporization Methods 0.000 abstract description 3
- 230000008016 vaporization Effects 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract 1
- 230000011218 segmentation Effects 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 238000004375 physisorption Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- 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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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Abstract
The invention discloses a kind of system and method for automatic control autoclave heating cooling, system is mainly made of heating system and cooling system.Heating system mainly includes steam inlet pipeline, heating regulating valve, heat preservation regulating valve, jacket outlet pipeline, knockout drum, condensation-water drain pipeline, condensation-water drain regulating valve；Cooling system mainly includes recirculated water suction line, recirculated water entry switch valve, circulating water outlet pipeline, circulating water outlet regulating valve, special water inlet pipeline, special water inlet switch valve, special water outlet line, special water out regulating valve.This system is guaranteed speed and the time of heating, is guaranteed the accurate adjusting of holding stage temperature using heating regulating valve and heat preservation regulating valve bivalve control；Using special water and recirculated water segmentation automatic adjustment cooling, guarantee the stabilization of the constant and product quality of crystallization temperature fall time.Special water can reduce the noise that cooling vaporization generates, and play the role of cleaning reacting kettle jacketing, prevent collet fouling and influence heat-transfer effect.
Description
Technical field
The present invention relates to a kind of system and methods of automatic control autoclave heating cooling.
Background technique
The working principle of reaction kettle is to be put into action solvent in internal layer to be stirred to react, and interlayer can lead to different cold and hot
Do circulating-heating or cooling reaction in source.By reaction kettle interlayer, the thermosol media or cooling media of constant temperature are injected, in reaction kettle
Material carry out heated at constant temperature or refrigeration.
Designer is found in many engineerings at home in the selection of heating regulating valve, when especially selecting regulating valve bore
There are random phenomenon is more serious.Heating and thermal insulation uses one regulating valve of some designers simultaneously, if selection regulating valve
Bore is less than normal, causes heating speed very slow, if selected, regulating valve bore is bigger than normal so that control performance is deteriorated, and will lead to heating end
Section and holding stage temperature are difficult to adjust, and temperature is unstable, and the operation of regulating valve long-time small guide vane can damage spool.
Many users are using directly logical recirculated water or refrigerant cooling in temperature-fall period, and use for a long time can be to kettle in this way
Service life influence very big, and reaction higher for temperature, directly logical recirculated water or refrigerant cooling can generate a large amount of
Steam generates very big noise, using the meeting fouling of a period of time kettle collet, is difficult to clean up, and will affect heat-transfer effect.Exist simultaneously
In temperature-fall period, the flow velocity and temperature fall time of water are not controlled, in this way for many synthetic reactions cooling crystallization process, product matter
The repeatability of amount is difficult to control.
To solve the above-mentioned problems, the present invention proposes that a kind of automatic control autoclave heats system and the side of cooling
Method, come guarantee heating speed and the time, the accurate adjusting of temperature, the stabilization of the constant and product quality of crystallization temperature fall time,
Reduce the noise that cooling vaporization generates, prevents reacting kettle jacketing fouling and influence heat-transfer effect, improve the service life of reaction kettle
It is essential.
Summary of the invention
The present invention provides a kind of system of automatic control autoclave heating cooling, and system is mainly by heating system and drop
Warm system composition.
The autoclave 5 is equipped with reacting kettle jacketing 6 and temperature controller 13.The reacting kettle jacketing 6 is equipped with steam
Entrance 23, condensation-water drain 24, cooling water inlet 25, cooling water outlet 26.
The heating system mainly includes steam inlet pipeline 1, heating regulating valve 2, heat preservation regulating valve 3, jacket outlet pipe
Line 7, knockout drum 8, condensation-water drain pipeline 12, condensation-water drain regulating valve 11.The steam inlet pipeline 1 enters with steam
Mouth 23 is connected, and the heating regulating valve 2 and heat preservation 3 parallel connection of regulating valve are located on steam inlet pipeline 1, the jacket outlet pipeline
7 are connected with condensation-water drain 24,8 entrance of knockout drum respectively, the outlet of knockout drum 8 and condensation-water drain pipeline 12
It is connected, the condensation-water drain pipeline 12 is equipped with condensation-water drain regulating valve 11.
The cooling system mainly includes recirculated water suction line 14, recirculated water entry switch valve 15, circulating water outlet pipe
Line 16, circulating water outlet regulating valve 17, special water inlet pipeline 18, special water inlet switch valve 19, special water outlet line 20,
Special water out regulating valve 21.The recirculated water suction line 14 and special water inlet pipeline 18 respectively with 25 phase of cooling water inlet
Even, the recirculated water entry switch valve 15 and special water inlet switch valve 19 are respectively provided at recirculated water suction line 14 and special water
On suction line 18；The circulating water outlet pipeline 16 and special water outlet line 20 are connected with cooling water outlet 26 respectively, institute
It states circulating water outlet regulating valve 17 and special water out regulating valve 21 is respectively provided at circulating water outlet pipeline 16 and special water out
On pipeline 20.
Further, in the above-mentioned technical solutions, pressure gauge 4, the steam inlet tube are equipped with before the steam inlet 23
Balance pipeline 9 is equipped between line 1 and knockout drum 8, the knockout drum 8 is equipped with fluid level controller 10, the liquid level control
Device 10 processed is interlocked with condensation-water drain regulating valve 11.
Further, in the above-mentioned technical solutions, the heating regulating valve 2, heat preservation regulating valve 3, recirculated water entry switch
Valve 15, special water inlet switch valve 19, circulating water outlet regulating valve 17, special water out regulating valve 21 respectively with temperature controller
13 interlockings.
Further, in the above-mentioned technical solutions, the heating regulating valve 2 is the mouth to match with steam inlet pipeline 1
The biggish regulating valve of diameter, heating the ratio between control valve stand diameter and steam inlet pipeline diameter are 0.5~1:1, and the heat preservation is adjusted
Saving valve 3 is the much smaller regulating valve of bore compared with steam inlet pipeline 1.The heat preservation control valve stand diameter and steam inlet
The ratio between pipeline diameter is 0.05~0.2:1.
Further, in the above-mentioned technical solutions, the special water is the softened water through being overpressurized.
Further, in the above-mentioned technical solutions, discharging valve door 22 is equipped with before the cooling water inlet 25.
Further, in the above-mentioned technical solutions, the condensation-water drain 24, cooling water outlet 25 are separately positioned on reaction
6 lower end of kettle collet.
The present invention provides a kind of method of automatic control autoclave heating cooling, using above-mentioned apparatus, including it is following
Step:
1. material is put into autoclave 5, stirring is opened, 2~6h of heating time, reaction are set in DCS system
150~200 DEG C of temperature, 48~96h of soaking time, 1~5h of temperature fall time open heating schedule, and steam is by steam inlet pipeline 1
Into reacting kettle jacketing 6, steam condensate (SC) enters knockout drum 8, condensation-water drain regulating valve 11 by jacket outlet pipeline 7
The rate of discharge that condensed water is controlled by fluid level controller 10 adjusts heating 2 aperture of regulating valve by temperature controller 13 to control
The rate of heat addition, when temperature is raised to 145~195 DEG C, heating regulating valve 2 is automatically closed, while opening heat preservation regulating valve 3, is passed through
Heat preservation regulating valve 3 adjusts temperature and is raised to 150~200 DEG C, keeps the temperature 48~96h h.
2. heat preservation regulating valve 3 and condensation-water drain regulating valve 11 is automatically closed, while opening spy after soaking time
Different water inlet switch valve 19 and special water out regulating valve 21, special water enter reacting kettle jacketing by special water inlet pipeline 18
6 start to cool down, and adjust special 21 aperture of water out regulating valve by temperature controller 13 to control rate of temperature fall, when temperature drops to
At 100 DEG C, special water inlet switch valve 19 and special water out regulating valve 21 is automatically closed, opens simultaneously recirculated water entry switch
Valve 15 and circulating water outlet regulating valve 17 adjust 17 aperture of circulating water outlet regulating valve by temperature controller 13 to control cooling speed
Recirculated water entry switch valve 15 and circulating water outlet regulating valve 19 is automatically closed when temperature is down to 50 DEG C in rate, opens discharging valve
Door 22 releases the recirculated water in collet.
Good effect using the above scheme: present system guarantees that the speed of heating and time, the accurate adjusting of temperature is brilliant
Change the stabilization of the constant and product quality of temperature fall time, reduce the noise of cooling vaporization generation, prevent reacting kettle jacketing fouling and
Heat-transfer effect is influenced, the service life of reaction kettle is improved.
Detailed description of the invention
This patent is further described with reference to the accompanying drawings and embodiments:
Attached drawing 1 is whole process schematic diagram of the present invention.
In figure: 1 steam inlet pipeline, 2 heating regulating valves, 3 heat preservation regulating valves, 4 pressure gauges, 5 autoclaves, 6 reactions
Kettle collet, 7 jacket outlet pipelines, 8 knockout drums, 9 balance pipelines, 10 fluid level controllers, 11 condensation-water drain regulating valves, 12
Condensation-water drain pipeline, 13 temperature controllers, 14 recirculated water suction lines, 15 recirculated water entry switch valves, 16 circulating water outlets
Pipeline, 17 circulating water outlet regulating valves, 18 special water inlet pipelines, 19 special water inlet switch valves, 20 special water outlet lines,
21 special water out regulating valves, 22 discharging valve doors, 23 steam inlets, 24 condensation-water drains, 25 cooling water inlets, 26 cooling waters go out
Mouthful.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings, but protection scope of the present invention is not limited to described in embodiment
Content.
As shown in Figure 1, a kind of system for automatically controlling autoclave heating cooling, system is mainly by heating system and drop
Warm system composition.
The autoclave 5 is equipped with reacting kettle jacketing 6 and temperature controller 13.The reacting kettle jacketing 6 is equipped with steam
Entrance 23, condensation-water drain 24, cooling water inlet 25, cooling water outlet 26.
The heating system mainly includes steam inlet pipeline 1, heating regulating valve 2, heat preservation regulating valve 3, jacket outlet pipe
Line 7, knockout drum 8, condensation-water drain pipeline 12, condensation-water drain regulating valve 11.The steam inlet pipeline 1 enters with steam
Mouth 23 is connected, and the heating regulating valve 2 and heat preservation 3 parallel connection of regulating valve are located on steam inlet pipeline 1, the jacket outlet pipeline
7 are connected with condensation-water drain 24,8 entrance of knockout drum respectively, the outlet of knockout drum 8 and condensation-water drain pipeline 12
It is connected, the condensation-water drain pipeline 12 is equipped with condensation-water drain regulating valve 11.
The cooling system mainly includes recirculated water suction line 14, recirculated water entry switch valve 15, circulating water outlet pipe
Line 16, circulating water outlet regulating valve 17, special water inlet pipeline 18, special water inlet switch valve 19, special water outlet line 20,
Special water out regulating valve 21.The recirculated water suction line 14 and special water inlet pipeline 18 respectively with 25 phase of cooling water inlet
Even, the recirculated water entry switch valve 15 and special water inlet switch valve 19 are respectively provided at recirculated water suction line 14 and special water
On suction line 18；The circulating water outlet pipeline 16 and special water outlet line 20 are connected with cooling water outlet 26 respectively, institute
It states circulating water outlet regulating valve 17 and special water out regulating valve 21 is respectively provided at circulating water outlet pipeline 16 and special water out
On pipeline 20.
It is equipped with pressure gauge 4 before the steam inlet 23, is equipped between the steam inlet pipeline 1 and knockout drum 8 flat
Weigh pipeline 9, and the knockout drum 8 is equipped with fluid level controller 10, the fluid level controller 10 and condensation-water drain regulating valve 11
Interlocking.
The heating regulating valve 2, recirculated water entry switch valve 15, special water inlet switch valve 19, is followed heat preservation regulating valve 3
Ring water out regulating valve 17, special water out regulating valve 21 are interlocked with temperature controller 13 respectively.
2 valve-seat diameter of heating regulating valve and 1 diameter ratio of steam inlet pipeline are 0.8:1, the heat preservation regulating valve 3
Valve-seat diameter and 1 diameter ratio of steam inlet pipeline are 0.1:1.
The special water is the softened water through being overpressurized.
Discharging valve door 22 is equipped with before the cooling water inlet 25.
The condensation-water drain 24, cooling water outlet 25 are separately positioned on 6 lower end of reacting kettle jacketing.
It, will be using the 8m of this system for the stability for detecting the system production product quality3Autoclave number be device
1；It will be using the 15m of this system3Autoclave number be device 2；Will steam directly commonly be controlled with a heating regulating valve
Heating and thermal insulation directly uses the 8m of circulating water cooling3High-pressure kettle system number is device 3；It will commonly directly be adjusted with a heating
It saves valve and controls steam heating and thermal insulation, directly use the 15m of circulating water cooling3High-pressure kettle system number is device 4.It is synthesized below
SSZ-13 exclusion experiments.
Embodiment 1
It is as follows using a kind of above-mentioned process for the system operatio for automatically controlling autoclave heating cooling:
By in SSZ-13 synthesis material investment device 1, stirring is opened, heating time 3h, reaction temperature are set in DCS system
165 DEG C, soaking time 72h, temperature fall time 4h are spent, heating schedule is opened, 1.6MPa steam is entered by steam inlet pipeline 1 to react
Kettle collet 6, steam condensate (SC) enter knockout drum 8 by jacket outlet pipeline 7, and condensation-water drain regulating valve 11 passes through liquid level
Controller 10 controls the rate of discharge of condensed water, controls the rate of heat addition by the adjusting of temperature controller 13 heating 2 aperture of regulating valve,
When temperature is raised to 160 DEG C, heating regulating valve 2 is automatically closed, while opening heat preservation regulating valve 3, is adjusted by heat preservation regulating valve 3
Temperature is raised to 165 DEG C, keeps the temperature 72h.
After soaking time, heat preservation regulating valve 3 and condensation-water drain regulating valve 11 is automatically closed, at the same open it is special
Water inlet switch valve 19 and special water out regulating valve 21, special water (using the softened water of 1.0MPa) pass through special water inlet pipe
Line 18 starts to cool down into reacting kettle jacketing 6, adjusts special 21 aperture of water out regulating valve by temperature controller 13 to control drop
When temperature drops to 100 DEG C special water inlet switch valve 19 and special water out regulating valve 21 is automatically closed, simultaneously in warm rate
Recirculated water entry switch valve 15 and circulating water outlet regulating valve 17 are opened, circulating water outlet regulating valve is adjusted by temperature controller 13
17 apertures control rate of temperature fall, when temperature is down to 50 DEG C, recirculated water entry switch valve 15 and circulating water outlet are automatically closed
Regulating valve 19 opens the recirculated water in the releasing collet of discharging valve door 22.Experiment is repeated twice using the device same experimental conditions.
Testing separately sampled number three times is 1,2,3.
Embodiment 2
Operating procedure is same as Example 1, and difference is that device 1 changes device 2 into, and testing separately sampled number three times is 4,
5,6。
Comparative example 1
By in SSZ-13 synthesis material investment device 3, stirring is opened, heating schedule is opened, adjusts heating control valve opening
The rate of heat addition is controlled, until keeping the temperature 72h when temperature rises to 165 DEG C.After soaking time, heating regulating valve is closed, is led to
Circulating water cooling closes recirculated water when temperature is down to 50 DEG C, releases the recirculated water in collet.Using the device identical experiment
Condition is repeated twice experiment.Testing separately sampled number three times is 7,8,9.
Comparative example 2
Operating procedure is identical as comparative example 1, and difference is that device 3 changes device 4 into, tests separately sampled number three times and is
10,11,12。
Embodiment 3
Characterization point is carried out using 2020 type nitrogen physisorption instrument of Micromeritics ASAP to 1~12 sample of number
Analysis.The preprocess method of sample is as follows before analysis: at normal temperature by sieve sample vacuumize process, when reaching vacuum condition
Afterwards, in 120 DEG C of processing 2h；Later in 330 DEG C of processing 2h.The results are shown in Table 1 for nitrogen physisorption.
| Sample number into spectrum | I grades of mesoporous average value/nm | II grades of mesoporous average value/nm | Micro pore volume/ml | Mesopore volume/ml | Specific surface area/(m2/g) |
| 1 | 3.6 | 10.5 | 0.26 | 0.40 | 489.7 |
| 2 | 3.3 | 11.2 | 0.25 | 0.39 | 485.6 |
| 3 | 3.5 | 10.8 | 0.26 | 0.38 | 484.9 |
| 4 | 3.7 | 11.5 | 0.27 | 0.39 | 483.4 |
| 5 | 3.8 | 10.7 | 0.25 | 0.38 | 486.0 |
| 6 | 3.6 | 11.0 | 0.24 | 0.39 | 482.3 |
| 7 | 4.2 | 7.9 | 0.23 | 0.42 | 467.2 |
| 8 | 3.6 | 9.5 | 0.26 | 0.37 | 481.3 |
| 9 | 5.3 | 10.8 | 0.20 | 0.34 | 475.6 |
| 10 | 4.4 | 12.3 | 0.22 | 0.36 | 471.3 |
| 11 | 3.5 | 9.7 | 0.27 | 0.44 | 482.8 |
| 12 | 2.7 | 11.4 | 0.21 | 0.41 | 463.4 |
Embodiment 4
Tabletting is carried out to 1~12 sample molecule of number sieve original powder, is crushed to 20~40 mesh.It weighs 1g sample and is packed into fixed bed
Reactor carries out MTO evaluation.Lead to nitrogen activation 2h at 550 DEG C, is then cooled to 450 DEG C.Methanol is carried by nitrogen, nitrogen
Flow velocity is 18ml/min, methanol weight air speed 5h-1.Obtained product is divided by online gas-chromatography (Agilent7890)
It analyses, as a result (t50: conversion ratio was reduced to for 50% time experienced from 100%；t98: conversion ratio is reduced to 98% institute from 100%
The time of experience) it is shown in Table 2.
The sample mesoporous pore size of number 1~6, structure, volume, specific surface area repeatability are above volume as can be seen from Table 1
Numbers 7~12 sample.The sample of number 1~6 selectivity and conversion ratio repeatability in MTO reaction is high as can be seen from Table 2
In number 7~12 sample.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of system for automatically controlling autoclave heating cooling, it is characterised in that: system is mainly by heating system and drop
Warm system composition；
The autoclave is equipped with reacting kettle jacketing and temperature controller；The reacting kettle jacketing is equipped with steam inlet, condensation
Water out, cooling water inlet, cooling water outlet；
The heating system mainly includes steam inlet pipeline, heating regulating valve, heat preservation regulating valve, jacket outlet pipeline, gas-liquid
Knockout drum, condensation-water drain pipeline, condensation-water drain regulating valve；The steam inlet pipeline is connected with steam inlet, described to add
Heat regulating valve and heat preservation regulating valve parallel connection be located on the pipeline of steam inlet, the jacket outlet pipeline respectively with condensation-water drain,
Knockout drum entrance is connected, and the knockout drum outlet is connected with condensation-water drain pipeline, the condensation-water drain pipeline
Equipped with condensation-water drain regulating valve；
The cooling system mainly includes recirculated water suction line, recirculated water entry switch valve, circulating water outlet pipeline, recirculated water
Index combustion fan, special water inlet pipeline, special water inlet switch valve, special water outlet line, special water out regulating valve；Institute
It states recirculated water suction line and special water inlet pipeline is connected with cooling water inlet respectively, the recirculated water entry switch valve and spy
Different water inlet switch valve is respectively provided on recirculated water suction line and special water inlet pipeline；The circulating water outlet pipeline and spy
Different water outlet line is connected with cooling water outlet respectively, and the circulating water outlet regulating valve and special water out regulating valve are set respectively
On circulating water outlet pipeline and special water outlet line.
2. a kind of system for automatically controlling autoclave heating cooling according to claim 1, it is characterised in that: described
It is equipped with pressure gauge before steam inlet, balance pipeline, the gas-liquid point are equipped between the steam inlet pipeline and knockout drum
It is equipped with fluid level controller from tank, the fluid level controller and condensation-water drain regulating valve interlock.
3. a kind of system for automatically controlling autoclave heating cooling according to claim 1, it is characterised in that: described
Heat regulating valve, heat preservation regulating valve, recirculated water entry switch valve, special water inlet switch valve, circulating water outlet regulating valve, special
Water out regulating valve is interlocked with temperature controller respectively.
4. a kind of system for automatically controlling autoclave heating cooling according to claim 1, it is characterised in that: heating
The ratio between control valve stand diameter and steam inlet pipeline diameter are 0.5~1:1, and the heat preservation control valve stand diameter enters with steam
The ratio between mouth pipeline diameter is 0.05~0.2:1.
5. a kind of system for automatically controlling autoclave heating cooling according to claim 1, it is characterised in that: described
Special water is the softened water through being overpressurized.
6. a kind of system for automatically controlling autoclave heating cooling according to claim 1, it is characterised in that: described
Discharging valve door is equipped with before cooling water inlet.
7. a kind of system for automatically controlling autoclave heating cooling according to claim 1, it is characterised in that: described
Condensation-water drain, cooling water outlet are separately positioned on reacting kettle jacketing lower end.
8. a kind of method for automatically controlling autoclave heating cooling, it is characterised in that: use claim 1-7 any one
The device, comprising the following steps:
1. material is put into autoclave, stirring is opened, 2~6h of heating time, reaction temperature are set in DCS system
150~200 DEG C, 48~96h of soaking time, 1~5h of temperature fall time, open heating schedule, and steam is entered by steam inlet pipeline
Reacting kettle jacketing, steam condensate (SC) enter knockout drum by jacket outlet pipeline, and condensation-water drain regulating valve passes through liquid level
Controller controls the rate of discharge of condensed water, adjusts heating control valve opening by temperature controller to control the rate of heat addition, works as temperature
When degree is raised to 145~195 DEG C, heating regulating valve is automatically closed, while opening heat preservation regulating valve, adjusts valve regulation temperature by heat preservation
Degree is raised to 150~200 DEG C, keeps the temperature 48~96h；
2. heat preservation regulating valve and condensation-water drain regulating valve is automatically closed, while opening special water and entering after soaking time
Mouth switch valve and special water out regulating valve, special water enter reacting kettle jacketing by special water inlet pipeline and start to cool down, by
Temperature controller adjusts special water out control valve opening to control rate of temperature fall, and when temperature drops to 100 DEG C, spy is automatically closed
Different water inlet switch valve and special water out regulating valve, open simultaneously recirculated water entry switch valve and circulating water outlet regulating valve,
Circulating water outlet control valve opening is adjusted to control rate of temperature fall by temperature controller, when temperature is down to 50 DEG C, is automatically closed
Recirculated water entry switch valve and circulating water outlet regulating valve open the recirculated water in discharging valve door releasing collet.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110694564A (en) * | 2019-11-14 | 2020-01-17 | 清远市番亿聚氨酯有限公司 | Temperature control system of polyurethane reaction kettle |
| CN112083141A (en) * | 2020-09-08 | 2020-12-15 | 西南石油大学 | Cement paste/drilling fluid hydration heat-affected natural gas hydrate stability testing device |
| CN112466488A (en) * | 2020-11-13 | 2021-03-09 | 南华大学 | CPR1000 nuclear power unit SG simulation device and method |
| CN113813876A (en) * | 2021-10-13 | 2021-12-21 | 长春市吉达自动化系统有限公司 | Sorbitol production system based on full-automatic control by temperature change and pressure-controlled reation kettle |
| CN114115143A (en) * | 2021-11-08 | 2022-03-01 | 东力（南通）化工有限公司 | Method for automatically controlling methyl hydrazine production process through DCS |
| CN114534651A (en) * | 2022-01-13 | 2022-05-27 | 宁夏天霖新材料科技有限公司 | Reactor temperature control method |
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| CN107930563A (en) * | 2017-12-25 | 2018-04-20 | 杭州普适自动化工程有限公司 | A kind of temperature of reaction kettle control system and method |
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|---|---|---|---|---|
| CN107930563A (en) * | 2017-12-25 | 2018-04-20 | 杭州普适自动化工程有限公司 | A kind of temperature of reaction kettle control system and method |
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Application publication date: 20190830 |