CN112083739A - Safety control method for oxygen content in tail gas of epoxy chloropropane process - Google Patents
Safety control method for oxygen content in tail gas of epoxy chloropropane process Download PDFInfo
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000001301 oxygen Substances 0.000 title claims abstract description 83
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000007789 gas Substances 0.000 title claims abstract description 27
- 230000008569 process Effects 0.000 title claims abstract description 22
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 title claims abstract description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 49
- OWXJKYNZGFSVRC-NSCUHMNNSA-N (e)-1-chloroprop-1-ene Chemical compound C\C=C\Cl OWXJKYNZGFSVRC-NSCUHMNNSA-N 0.000 claims abstract description 37
- 239000003054 catalyst Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000011261 inert gas Substances 0.000 claims abstract description 23
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 13
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 238000006735 epoxidation reaction Methods 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 42
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 238000011897 real-time detection Methods 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 abstract description 16
- 238000004880 explosion Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 35
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002808 molecular sieve Substances 0.000 description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 5
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- XEPXTKKIWBPAEG-UHFFFAOYSA-N 1,1-dichloropropan-1-ol Chemical compound CCC(O)(Cl)Cl XEPXTKKIWBPAEG-UHFFFAOYSA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005422 blasting Methods 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007127 saponification reaction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 description 1
- SNIOPGDIGTZGOP-UHFFFAOYSA-N Nitroglycerin Chemical compound [O-][N+](=O)OCC(O[N+]([O-])=O)CO[N+]([O-])=O SNIOPGDIGTZGOP-UHFFFAOYSA-N 0.000 description 1
- 239000000006 Nitroglycerin Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229920005558 epichlorohydrin rubber Polymers 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 229960003711 glyceryl trinitrate Drugs 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D11/00—Control of flow ratio
- G05D11/02—Controlling ratio of two or more flows of fluid or fluent material
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Automation & Control Theory (AREA)
- Epoxy Compounds (AREA)
Abstract
The invention relates to the field of chemical safety, and discloses a safety control method for oxygen content in tail gas of an epichlorohydrin process. The method is used for synthesizing epichlorohydrin by direct epoxidation of chloropropene in the presence of a catalyst, and comprises the following steps: detecting the volume concentration of gas-phase oxygen in the reactor; and controlling the filling of inert gas when the detected volume concentration of the gas-phase oxygen in the reactor exceeds an alarm value, so that the oxygen concentration is reduced to be below the alarm value and/or the detected volume concentration of the gas-phase oxygen in the reactor exceeds an interlocking value, and cutting off the feeding of hydrogen peroxide and chloropropene. When the method is used for synthesizing epoxy chloropropane by directly epoxidizing chloropropene in the presence of a catalyst, the oxygen content of reaction tail gas can be better controlled, the occurrence of gas phase explosion is prevented, the safe and stable operation of the device is ensured, and a better technical effect is obtained.
Description
Technical Field
The invention relates to the field of chemical safety, in particular to a safety control method for oxygen content in tail gas of an epichlorohydrin process.
Background
Epichlorohydrin is an important organic chemical raw material and is mainly used for synthesizing various products such as epoxy resin, glycerin, epichlorohydrin rubber, nitroglycerin explosive and the like.
The main industrial production method of epichlorohydrin is chloropropene method, which accounts for more than 90% of the global epichlorohydrin production capacity, and the process comprises 3 main steps of chloropropene preparation by chlorination of propylene, hypochlorination of chloropropene to generate dichloropropanol and saponification of dichloropropanol to synthesize epichlorohydrin. At present, in order to realize the greening of the production process of epoxy chloropropane, two reaction steps of chlorohydrination and saponification which mainly generate wastewater and waste residue are removed, and 3-chloropropene (chloropropene for short) is directly epoxidized to synthesize the epoxy chloropropane by one-step reaction, so that the discharge amount of the wastewater is remarkably reduced, and meanwhile, calcium chloride waste residue is not generated.
The new technology for synthesizing epoxy chloropropane by directly epoxidizing chloropropene is characterized by using chloropropene, ammonia and hydrogen peroxide as solvents under the condition of low pressure and adopting titanium-silicon molecular sieve catalyst (hereinafter referred to as catalyst) to synthesize epoxy chloropropane in one step in a fixed bed tubular reactor, and the chemical reaction equation is as follows:
ClCH2CH＝CH2+H2O2→ClCH2CHOCH2+H2O (1)
compared with the traditional preparation process, the process for directly synthesizing the epichlorohydrin greatly shortens the process flow, has the advantages of mild reaction conditions, high selectivity and conversion rate, no byproduct calcium chloride waste residue, reduction of wastewater discharge, higher technical economy and environmental protection benefit, and is expected to replace the traditional generation process.
However, since the reaction process involves hydrogen peroxide, in addition to the main reaction, a side reaction of decomposition of hydrogen peroxide may occur:
2H2O2→2H2O+O2↑ (2)
the hydrogen peroxide is easy to decompose in the reaction process to release oxygen, and the oxygen generated in the subsequent separation process of the reaction is mixed with combustible gases such as epichlorohydrin, chloropropene, methanol and the like to cause explosion risks.
Therefore, it is urgently needed to provide a safe control method for oxygen content in tail gas in the process of synthesizing epichlorohydrin by directly epoxidizing chloropropene in the presence of a catalyst.
Disclosure of Invention
The invention aims to overcome the problem of poor safety in the prior art, and provides a safe control method for the oxygen content in the tail gas of an epichlorohydrin process.
In order to achieve the above object, the present invention provides a method for safely controlling the oxygen content in the tail gas of an epichlorohydrin process, which is used for the direct epoxidation of chloropropene to epichlorohydrin in the presence of a catalyst, and comprises the following steps:
detecting the volume concentration of gas-phase oxygen in the reactor; and
controlling the filling of inert gas when the detected volume concentration of gas-phase oxygen in the reactor exceeds an alarm value, so that the volume concentration of oxygen is reduced to be below the alarm value and/or
And cutting off the feed of hydrogen peroxide and chloropropene when the detected volume concentration of gas-phase oxygen in the reactor exceeds an interlocking value.
In the control method, a catalyst is used in the process of synthesizing epichlorohydrin by directly epoxidizing chloropropene, and the whole process keeps methanol circulation.
Optionally, when the detected volume concentration of the gas-phase oxygen in the reactor exceeds an interlocking value, the feed of hydrogen peroxide and chloropropene is cut off, and inert gas is filled into the reactor simultaneously, so that the volume concentration of the oxygen is reduced to be below an alarm value.
Optionally, the alarm value is greater than or equal to 2 vol% and less than 4 vol%.
Optionally, the oxygen volume concentration is reduced to less than 2 vol% after the inert gas is introduced.
Optionally, the interlock value is 4 to 7 volume%.
Optionally, the hydrogen peroxide and chloropropene feeds are cut off while inert gas is introduced so that the oxygen concentration is reduced to less than 4 volume percent, preferably less than 2 volume percent.
Optionally, the catalyst is added in an amount of 3 to 5 wt% based on the total weight of the reactants.
Optionally, the catalyst is a silicon-titanium molecular sieve catalyst.
Optionally, the reactor is a fixed bed tubular reactor.
Optionally, the oxidation reaction conditions include: the reaction temperature is 40-100 ℃, the reaction pressure is 0.1-0.4MPa, and the space velocity of the catalytic oxidation reaction is 1000-3000h-1。
Optionally, the inert gas is nitrogen and/or argon, preferably nitrogen.
Optionally, the volume concentration of the gas-phase oxygen in the detection reactor is detected in real time.
By the technical scheme, the safety control condition of the oxygen content in the tail gas in the process of synthesizing the epoxy chloropropane by directly epoxidizing chloropropene in the presence of the catalyst is determined, so that the occurrence of gas-phase combustion and explosion accidents can be effectively avoided, and the safe and stable operation of the device is ensured.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The inventor of the invention finds out through experiments that the change rule of oxygen in the tail gas of the process of synthesizing epoxy chloropropane by directly epoxidizing chloropropene in the presence of a catalyst and determines the safe control condition of the oxygen content in the tail gas, and can effectively avoid the occurrence of gas-phase explosion accidents and ensure the safe and stable operation of the device through the control condition, thereby completing the invention.
The invention provides a safe control method of oxygen content in tail gas of an epoxy chloropropane process, which is used for synthesizing epoxy chloropropane by directly epoxidizing chloropropene in the presence of a catalyst, and comprises the following steps:
detecting the volume concentration of gas-phase oxygen in the reactor; and
controlling the filling of inert gas when the detected volume concentration of gas-phase oxygen in the reactor exceeds an alarm value, so that the volume concentration of oxygen is reduced to be below the alarm value and/or
And cutting off the feed of hydrogen peroxide and chloropropene when the detected volume concentration of gas-phase oxygen in the reactor exceeds an interlocking value.
In the control method, a catalyst is used in the process of synthesizing epichlorohydrin by directly epoxidizing chloropropene, and the whole process keeps methanol circulation.
Optionally, when the detected volume concentration of the gas-phase oxygen in the reactor exceeds an interlocking value, the feed of hydrogen peroxide and chloropropene is cut off, and inert gas is filled into the reactor simultaneously, so that the volume concentration of the oxygen is reduced to be below an alarm value.
Optionally, the alarm value is greater than or equal to 2 vol% and less than 4 vol%.
Optionally, the oxygen volume concentration is reduced to less than 2 vol% after the inert gas is introduced. For example, when the alarm value is set to 3 vol%, the detected volume concentration of the gas-phase oxygen in the reactor is 3.5 vol%, and the concentration exceeds the alarm value, the filling of the inert gas is controlled, so that the volume concentration of the oxygen is reduced to be less than 3 vol%, the volume concentration of the gas-phase oxygen in the reactor is reduced, the occurrence of gas-phase explosion accidents is avoided, and the safe and stable operation of the device is ensured; or when the alarm value is set to be 3 volume percent, the detected volume concentration of the gas-phase oxygen in the reactor is 3.5 volume percent, the concentration exceeds the alarm value, and the filling of the inert gas is controlled, so that the volume concentration of the oxygen is reduced to be less than 2 volume percent, the volume concentration of the gas-phase oxygen in the reactor is reduced, the occurrence of gas-phase explosion accidents is avoided, and the safe and stable operation of the device is ensured.
Optionally, the interlock value is 4 to 7 volume%.
Optionally, the hydrogen peroxide and chloropropene feeds are cut off while inert gas is introduced so that the oxygen concentration is reduced to less than 4 volume percent, preferably less than 2 volume percent. For example, when the interlocking value is set to 5 vol%, the detected volume concentration of gas-phase oxygen in the reactor is 6 vol%, and exceeds the interlocking value, the filling of inert gas is controlled, the feeding of hydrogen peroxide and chloropropene is cut off, and simultaneously the inert gas is filled, so that the volume concentration of the oxygen is reduced to be less than 4 vol%, and by reducing the volume concentration of the gas-phase oxygen in the reactor, the occurrence of gas-phase explosion accidents is avoided, and the safe and stable operation of the device is ensured; or when the interlocking value is set to be 5 volume percent, the detected volume concentration of the gas-phase oxygen in the reactor is 6 volume percent and exceeds the interlocking value, the filling of the inert gas is controlled, the feeding of hydrogen peroxide and chloropropene is cut off, and the inert gas is filled simultaneously, so that the volume concentration of the oxygen is reduced to be less than 2 volume percent, the occurrence of gas-phase explosion accidents is avoided by reducing the volume concentration of the gas-phase oxygen in the reactor, and the safe and stable operation of the device is ensured.
Optionally, the catalyst is added in an amount of 3 to 5 wt% based on the total weight of the reactants.
Optionally, the catalyst is a silicon-titanium molecular sieve catalyst.
Optionally, the reactor is a fixed bed tubular reactor.
Optionally, the oxidation reaction conditions include: the reaction temperature is 40-100 ℃, the reaction pressure is 0.1-0.4MPa, and the space velocity of the catalytic oxidation reaction is 1000-3000h-1。
Optionally, the inert gas is nitrogen and/or argon, preferably nitrogen. Through letting in inert gas, dilute and inert to the oxygen in the reactor, further avoid the emergence of gaseous phase blasting accident, guarantee the safe and stable operation of device.
Optionally, the volume concentration of the gas-phase oxygen in the detection reactor is detected in real time. Through the oxygen volume concentration in the real-time detection reactor, the emergence of gas phase blasting accident is avoided more effectually, guarantees the safe steady operation of device.
The present invention will be described in detail below with reference to examples, but the present invention is not limited to the following examples.
Example 1
The method comprises the steps of synthesizing epichlorohydrin in one step in a fixed bed tubular reactor by adopting a titanium-silicon molecular sieve catalyst and methanol as a solvent and using chloropropene, ammonia and hydrogen peroxide. Wherein, the dosage of chloropropene, ammonia, hydrogen peroxide, titanium silicalite molecular sieve catalyst and methanol are respectively 11.6kg/hr, 0.005kg/hr, 2.1kg/hr, 0.62kg and 6.9kg/hr, and the reaction conditions in the reactor comprise: the reaction temperature is 40 ℃, the reaction pressure is 0.1MPa, and the space velocity of the catalytic oxidation reaction is 1000h-1And the methanol circulation is kept in the whole process.
The alarm value of the oxygen volume concentration in the reaction tail gas is set at 2 volume percent, and the interlocking value is set at 4 volume percent.
And arranging an oxygen detector in a gas phase space in the reactor to test the volume concentration of oxygen, starting a nitrogen regulating valve of the reactor when the measured volume concentration of the gas-phase oxygen in the reactor is 2.8 volume percent and exceeds an alarm value, filling nitrogen into the reactor, and stopping filling the nitrogen when the volume concentration of the oxygen is reduced to be less than 2 volume percent.
And when the measured volume concentration of the gas-phase oxygen in the reactor is 4 volume percent and reaches an interlocking value, the system immediately starts interlocking control measures to emergently cut off the feeding of the hydrogen peroxide and the chloropropene, and simultaneously fills nitrogen into the reactor, and stops nitrogen filling and starts the feeding of the hydrogen peroxide and the chloropropene until the volume concentration of the oxygen is reduced to be less than 2 volume percent, so as to ensure the continuous operation of the production process.
Example 2
The same reaction conditions as in example 1 were employed.
The alarm value of the oxygen volume concentration in the reaction tail gas is set at 2.5 volume percent, and the interlocking value is set at 4 volume percent.
And arranging an oxygen detector in a gas phase space in the reactor to test the volume concentration of oxygen, starting a nitrogen regulating valve of the reactor when the measured volume concentration of the gas-phase oxygen in the reactor is 3 volume percent and exceeds an alarm value, filling nitrogen into the reactor, and stopping filling the nitrogen when the volume concentration of the oxygen is reduced to be less than 2.5 volume percent.
And when the measured volume concentration of the gas-phase oxygen in the reactor is 4 volume percent and reaches an interlocking value, the system immediately starts an interlocking control measure to emergently cut off the feeding of the hydrogen peroxide and the chloropropene, and simultaneously fills nitrogen into the reactor, and stops nitrogen filling and starts the feeding of the hydrogen peroxide and the chloropropene until the volume concentration of the oxygen is reduced to be less than 2.5 volume percent, so that the continuous operation of the production process is ensured.
Example 3
The same reaction conditions as in example 1 were employed.
The alarm value of the oxygen volume concentration in the reaction tail gas is set at 3 volume percent, and the interlocking value is set at 4 volume percent.
And arranging an oxygen detector in a gas phase space in the reactor to test the volume concentration of oxygen, starting a nitrogen regulating valve of the reactor when the measured volume concentration of the gas-phase oxygen in the reactor is 3.5 volume percent and exceeds an alarm value, filling nitrogen into the reactor, and stopping filling the nitrogen when the volume concentration of the oxygen is reduced to be less than 2 volume percent.
And when the measured volume concentration of the gas-phase oxygen in the reactor is 4 volume percent and reaches an interlocking value, the system immediately starts an interlocking control measure to emergently cut off the feeding of the hydrogen peroxide and the chloropropene, and simultaneously fills nitrogen into the reaction gas until the volume concentration of the oxygen is reduced to less than 2 volume percent, stops the nitrogen filling, starts the feeding of the hydrogen peroxide and the chloropropene, and ensures the continuous operation of the production process.
The embodiment can show that: by adopting the control method provided by the invention, under the condition of using the catalyst, the epoxidation reaction condition can be effectively monitored, gas phase explosion caused by reaction deterioration is prevented, the safe and stable operation of the device is ensured, and a better technical effect is obtained.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A safety control method for oxygen content in tail gas of epoxy chloropropane process is used for synthesizing epoxy chloropropane by direct epoxidation of chloropropene in the presence of catalyst, and is characterized in that the method comprises the following steps:
detecting the volume concentration of gas-phase oxygen in the reactor; and
controlling the filling of inert gas when the detected volume concentration of gas-phase oxygen in the reactor exceeds an alarm value, so that the volume concentration of oxygen is reduced to be below the alarm value, and/or
And cutting off the feed of hydrogen peroxide and chloropropene when the detected volume concentration of gas-phase oxygen in the reactor exceeds an interlocking value.
2. The method of claim 1, wherein the detected gas phase oxygen volume concentration in the reactor exceeds an interlock value by shutting off the hydrogen peroxide and chloropropene feeds while introducing an inert gas such that the oxygen volume concentration falls below an alarm value.
3. The method according to claim 1, wherein the alarm value is ≥ 2% and < 4% by volume;
preferably, the inert gas is introduced such that the oxygen volume concentration is reduced to less than 2 volume percent.
4. The method of claim 1, wherein the interlock value is 4-7% by volume;
preferably, the hydrogen peroxide and chloropropene feeds are cut off while inert gas is fed in such that the oxygen concentration by volume is reduced to less than 4% by volume, more preferably less than 2% by volume.
5. The process of any of claims 1-4, wherein the catalyst is added in an amount of 3 to 5 wt.%, based on the total weight of the reactants.
6. The method of claim 5, wherein the catalyst is a titanium silicalite catalyst.
7. The process of any one of claims 1-4, wherein the reactor is a fixed bed shell and tube reactor;
preferably, the oxidation reaction conditions include: the reaction temperature is 40-100 ℃, the reaction pressure is 0.1-0.4MPa, and the space velocity of the catalytic oxidation reaction is 1000-3000h-1。
8. The method according to any one of claims 1-4, wherein the inert gas is nitrogen and/or argon, preferably nitrogen.
9. The method of any one of claims 1-4, wherein the detected gas phase oxygen volume concentration within the reactor is a gas phase oxygen volume concentration value at a plurality of sites.
10. The method of any one of claims 1-4, wherein the detecting the gas phase oxygen volume concentration within the reactor is a real-time detection.
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| CN114653317A (en) * | 2020-12-22 | 2022-06-24 | 中国石油化工股份有限公司 | Method for safely operating oxidative dehydrogenation reactor, oxidative dehydrogenation reaction device and application |
| CN114653170A (en) * | 2020-12-22 | 2022-06-24 | 中国石油化工股份有限公司 | Method and device for safe operation of tail gas absorption tower and application thereof |
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