CN109053647B - Production process for preparing maleic anhydride by oxidizing n-butane - Google Patents
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Abstract
The invention discloses a process for preparing maleic anhydride by oxidizing n-butane, belonging to the field of maleic anhydride production. The invention relates to a production process for producing maleic anhydride by oxidizing n-butane under lower operating pressure by improving the production process for preparing maleic anhydride by an original benzene oxidation method. In particular, the process adopts a self-made catalyst, so that the reaction has better selectivity and yield under the condition of low pressure, and simultaneously, the existing process is worked out and the cost is saved.
Description
Technical Field
The invention relates to the field of maleic anhydride production, in particular to a production process for producing maleic anhydride by using n-butane oxidation under lower operation pressure.
Background
Maleic anhydride is called maleic anhydride for short, and maleic anhydride is an important organic chemical raw material, is second only to phthalic anhydride and acetic anhydride, is the third largest organic anhydride in the world, and is widely used in the industries of petrochemical industry, food processing, medicines, building materials and the like. The method has the advantages of low raw material cost, relatively light pollution, high carbon atom utilization rate, low cis-anhydride production cost and the like, so that the technology for preparing the cis-anhydride by oxidizing the n-butane gradually becomes a main route of the cis-anhydride production and has a tendency of gradually replacing a benzene oxidation method. The domestic maleic anhydride production device by the benzene method is facing the examination of upgrading of a process route, the two routes mainly have the difference of production raw materials, operation conditions and an oxidation catalyst, benzene is adopted as a raw material by the benzene oxidation method, and the benzene and air are subjected to gas-phase oxidation reaction on the surface of a vanadium-molybdenum catalyst under the pressure of 0.05-0.06MPa to obtain reaction generated gas containing maleic anhydride; the n-butane oxidation method adopts n-butane as a raw material, and the n-butane and air generate gas phase oxidation reaction on the surface of a vanadium-phosphorus-oxygen catalyst under the pressure of 0.19-0.22MPa to obtain reaction generated gas containing maleic anhydride.
The two raw material routes must use catalysts of different systems, and the device for preparing maleic anhydride by the n-butane oxidation method can only use vanadium-phosphorus-oxygen catalysts. Because of the restriction of the operation condition of the catalyst, the existing vanadium phosphorus oxygen catalyst can not stably run on a production device for preparing maleic anhydride by a benzene oxidation method. Therefore, the prior device for preparing maleic anhydride by the benzene oxidation method is usually discarded. If the original benzene method device is reused by technical improvement and upgrading, the equipment utilization rate can be improved and the investment amount can be reduced. To meet this need, the present invention provides specific process improvements.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a technical scheme which is improved from a raw material route for preparing maleic anhydride by an orthobenzene oxidation method and is suitable for an n-butane oxidation method.
The production process for preparing maleic anhydride by benzene oxidation method is generally composed of units of a benzene storage tank, a fan, an air heater, an air-benzene mixer, a fixed bed reactor, a primary gas cooler, a partial cooler, an absorption tower, a rectification refining and tail gas burning device. Due to different storage conditions of liquid benzene and liquid n-butane, the process requires a newly-built liquid n-butane storage tank and a matched loading and unloading station. The following units are newly added in the improved process: the system comprises a normal butane storage tank, a normal butane evaporator and superheater, a trimethyl phosphate (TMP) adding system, an air-hydrocarbon mixer, a secondary gas cooler and a boiler water heater; the following units were modified: the fan (improve fan export pressure head), reactor outlet pipeline (change original carbon steel pipeline for the stainless steel), tail gas burn the device (change the heat carrier and increase the heat exchanger area), except need newly-increased and reform transform above-mentioned unit, need to change the vanadium phosphorus oxygen catalyst that possesses the operability under the low pressure condition.
The specific process steps for producing maleic anhydride by oxidizing n-butane after modification are as follows:
(1) liquid n-butane in the n-butane storage tank enters an n-butane evaporator, and is sent to an n-butane superheater after being heated and vaporized to obtain n-butane steam;
(2) pumping TMP into a TMP evaporator by a pump, mixing TMP steam by using nitrogen, and then feeding the mixed TMP steam into a normal butane pipeline to be mixed with butane steam in the step (1) to obtain organic steam;
(3) and (3) the air pressurized by the fan and heated by the air heater enters an air-hydrocarbon mixer to be mixed with the organic steam in the step (2), the obtained mixed gas enters a fixed bed tubular reactor filled with the catalyst together, the reacted gas enters a secondary gas cooler after passing through a primary gas cooler and then enters a partial cooler for cooling, the cooled reactant enters a crude anhydride separator, the gas enters an absorption tower, and the liquid crude anhydride enters a crude anhydride tank. Part of the anhydride entering the absorption tower is collected in an acid water tank after being washed by water, and finally the anhydride and the anhydride in the crude anhydride tank are refined together to obtain a maleic anhydride product.
In the step (1), the flow rate of n-butane is 0.09-0.10kg/Tube/h, the vaporization temperature of n-butane is 40-60 ℃, and the overheating temperature is 100-150 ℃.
In the step (3), the TMP concentration is 0.5-3.0ppm of the total volume of the inlet gas of the fixed bed tubular reactor.
The air flow rate in the step (3) is 2.0-2.1NCM/Tube/h, the pressurization pressure of the air at the outlet of the fan is 60-99 kPa through technical transformation, and the heating temperature is 150-180 ℃.
The preparation of maleic anhydride by n-butane oxidation is a strong exothermic reaction, the heat supply and heat transfer of the industrial reactor used in the invention are adjusted by molten salt formed after the mixture of sodium nitrite and potassium nitrate prepared in a certain proportion is melted, the reaction temperature is adjusted by adjusting the temperature of the molten salt (salt temperature for short),
in the step (3), the reaction pressure of the fixed bed is 60-99 kPa, the temperature of the molten salt is 405-415 ℃, and the temperature of the hot spot is 430-450 ℃. The generated gas at the outlet of the reactor comprises maleic anhydride, n-butane, oxygen, nitrogen and the mixed gas of the byproducts of carbon monoxide, carbon dioxide, acetic acid and acrylic acid.
In the step (3), the primary air cooler is cooled to 180-220 ℃, and the secondary air cooler is cooled to 145-165 ℃. The oxidation by-product acrylic acid is polymerized in the secondary gas cooler, so that two secondary gas coolers are required to be switched to ensure the continuous operation of the system. Meanwhile, in order to ensure the cooling temperature of the secondary air cooler, boiler water entering the secondary air cooler needs to be heated by a boiler and then enters the secondary air cooler, and the temperature of the boiler water at the outlet of the boiler water heater is 140-160 ℃.
The temperature of the mixed gas cooled by the middle cooler in the step (3) is 58-60 ℃, and the weight of the cooled liquid maleic anhydride accounts for 30-50%. If the cooler needs to be cleaned, the bypass can be switched to enter the absorption tower for water absorption, and the maleic anhydride is collected in the acid water tank in the form of maleic acid aqueous solution by using water as a solvent.
And (4) collecting maleic anhydride in the mixed gas entering the water absorption tower in the step (3) in the form of a maleic acid aqueous solution, and enabling n-butane, oxygen, nitrogen and oxidation byproducts, namely carbon monoxide and carbon dioxide, which do not participate in the reaction to enter a tail gas incinerator, incinerating and then emptying.
The catalyst selected by the invention can be the existing known catalyst applied to preparing maleic anhydride by oxidizing n-butane, and can also use the catalyst (NSMA-C4 SL-2 type catalyst for short) disclosed by the invention. The catalyst in the prior art can be used for preparing maleic anhydride by oxidizing n-butane, but the yield and the selectivity of the product are low, and long-period stable operation cannot be realized. The invention uses the NSMA-C4SL-2 type catalyst, not only has good selectivity and high yield of products, but also can realize long-period stable operation.
The NSMA-C4SL-2 type catalyst takes diatomite as a carrier, the weight content of the carrier is 20-40%, and the general formula of the active components is as follows: v 1.0PaMobOmWherein a is 0.8 to 1.5, b is 0.05 to 0.5, and m is the number of oxygen atoms required to satisfy the valence of each element.
The preparation method of the NSMA-C4SL-2 type catalyst comprises the following steps:
(1) dispersing 100-400 mesh diatomite into a mixed solution of isobutanol, benzyl alcohol and molybdenum isooctanoate, and reacting at 90-130 ℃ and a pressure of-5 to-30 Kpa to form a suspension;
(2) adding vanadium pentoxide and concentrated phosphoric acid into the suspension, depositing the generated precipitate on diatomite, filtering, drying at 100-150 ℃ for 4-24 h, and roasting at 200-400 ℃ for 1-8 h to form a precursor;
(3) and granulating the precursor into 10-60 meshes, tabletting the precursor into a hollow cylinder by using graphite as a lubricant, and activating the hollow cylinder at 400-500 ℃ for 10-20 h to obtain the catalyst.
By adopting the technical scheme provided by the invention, the following remarkable effects are achieved:
(1) the invention relates to a process for preparing maleic anhydride by oxidizing butane, which is improved on the basis of a production process flow of maleic anhydride by a benzene oxidation method.
(2) The process adopts the NSMA-C4SL-2 type catalyst, so that the maleic anhydride prepared by oxidizing n-butane has better selectivity and yield under the condition of low pressure, and the production profit is improved.
(3) If the improved process scheme is adopted, from the perspective of long-term operation industrial production, the price of n-butane is about 4000 yuan/ton, the price of petroleum benzene is about 6350 yuan/ton, and n-butane is about 2000 yuan/ton lower than the petroleum benzene, so that the cost can be saved, and better economic benefit can be brought.
Drawings
FIG. 1 is a block diagram of a benzene oxidation process;
FIG. 2 is a block diagram of a scheme of the reformed scheme suitable for preparing maleic anhydride by oxidation of n-butane.
Detailed Description
The invention is further illustrated by the following examples.
Example 1:
5500g of isobutanol, 1100g of benzyl alcohol and 63.2g of molybdenum isooctanoate are added into a reaction kettle with a stirring, heating and condensing reflux device, 720g of diatomite with the average particle size of 180 meshes is added after uniform stirring, the mixture is continuously stirred for 0.5h to obtain uniform suspension, the temperature is controlled to be 95 +/-5 ℃, the pressure is controlled to be minus 25 +/-5 kPa, 950g of 100 percent phosphoric acid is added into the reaction kettle within 1h at a constant speedAnd 860g of vanadium pentoxide, then continuously carrying out reflux reaction for 6h at the temperature and the pressure, cooling and filtering after the reaction is finished, drying the filter cake for 18h at the temperature of 130 +/-10 ℃, and then roasting for 8h at the temperature of 310 +/-10 ℃ to obtain the active precursor. Granulating the active precursor into 10-20 mesh particles, mixing with 4% (wt) graphite, tabletting into hollow cylinders with the outer diameter of 5mm, the inner diameter of 2.2mm and the height of 5mm, and activating at 470 +/-10 ℃ for 6h to obtain the catalyst with the composition V 1.0P1.0Mo0.1Om40% (wt) of diatomite and m is the number of oxygen atoms required to satisfy the valence of each element.
Example 2:
5000g of isobutanol, 1000g of benzyl alcohol and 48.5g of molybdenum isooctanoate are added into a reaction kettle with a stirring, heating and condensing reflux device, 486g of diatomite with the average particle size of 360 meshes is added after uniform stirring, uniform suspension is obtained after continuous stirring for 0.5h, the temperature is controlled to be 115 +/-5 ℃, the pressure is controlled to be 15 +/-5 kPa, 1000g of 100% phosphoric acid and 660g of vanadium pentoxide are added at a constant speed within 3h, then the reflux reaction is continuously carried out for 5h at the temperature and the pressure, cooling and filtering are carried out after the reaction is finished, a filter cake is dried for 20h at the temperature of 120 +/-10 ℃, and then the filter cake is roasted for 6h at the temperature of 310 +/-10 ℃ to obtain an active precursor. Granulating the active precursor into 10-20 mesh particles, mixing with 2% (wt) graphite, tabletting into hollow cylinders with outer diameter of 5mm, inner diameter of 2.2mm and height of 5mm, and activating at 470 +/-10 ℃ for 6h to obtain the catalyst with the composition V1.0P1.4Mo0.1Om33% (wt)/diatomite, and m is the number of oxygen atoms required to satisfy the valence of each element.
The process example comprises the following steps:
the reactors used in the following examples are fixed bed reactors, reaction tubes with equal length are 4000mm in length, the tube diameter of the reactor is 21mm, the catalyst adopts NSMA-C4SL-2 type catalyst, and the filling height is 3500 mm.
The following examples all use a ten thousand ton maleic anhydride production apparatus after the replacement process, as shown in fig. 2. Liquid n-butane in a butane storage tank enters a n-butane evaporator, the liquid n-butane is heated to 40-60 ℃ for vaporization and then sent to a n-butane superheater at 100-150 ℃ to obtain n-butane steam, TMP is pumped into the TMP evaporator through a pump, TMP steam is mixed with nitrogen and then enters a n-butane pipeline to be mixed with the n-butane steam to obtain organic steam, air which is pressurized to 60-99 kPa through a fan and then heated by an air heater at 150-180 ℃ enters an air-hydrocarbon mixer to be mixed with the organic steam, the obtained mixed gas enters a fixed bed tubular reactor filled with a catalyst together, the reacted gas is cooled to 180-220 ℃ through a primary gas cooler and then enters a secondary gas cooler at 145-165 ℃ to be cooled, wherein the temperature of the secondary air cooler is provided by boiler water at 140-160 ℃, the cooled reactant enters a crude anhydride separator, the gas enters an absorption tower, and the liquid crude anhydride enters a crude anhydride tank. Part of the acid anhydride entering the absorption tower is collected in an acid water tank after being washed by water, and finally the acid anhydride and the acid anhydride in the crude anhydride tank are refined together to obtain a maleic anhydride product.
Example 3:
the air flow is 2.05NCM/Tube/h, the n-butane flow is 0.096kg/Tube/h, the volume content of TMP is 1.5ppm, the inlet pressure of a reactor is 60kPaG, the molten salt temperature is 410 ℃, the hot spot temperature is 440 ℃, the n-butane conversion rate is 82.0 percent, the inventory is carried out after the stable operation of the device is carried out for 720 hours, the oxidation yield is 90 percent, the refining yield is 92 percent, the raw material consumption of each ton of products is 1.207t, the average price of the n-butane is 4000 yuan per ton, and the raw material cost of each ton of products is 4828 yuan; when the device takes benzene as a raw material route, the consumption of the raw materials of each ton of products is 1.150t, the average price of petroleum benzene is 6350 yuan per ton, and the cost of the raw materials of each ton of products is 7303 yuan; the raw material cost of the technically improved ton product is reduced by 2475 yuan.
Example 4:
air flow 2.05NCM/Tube/h, n-butane flow 0.096kg/Tube/h, TMP volume content 1.5ppm, reactor inlet pressure 90kPaG, molten salt temperature 405 ℃, hot spot temperature 435 ℃. The conversion rate of normal butane is 82.0 percent, the device is checked after being stably operated for 720 hours, the oxidation yield is 92 percent, the refining yield is 92 percent, the consumption of raw materials of each ton of products is 1.181t, the average price of normal butane is 4000 yuan per ton, and the cost of the raw materials of each ton of products is 4724 yuan; when the device takes benzene as a raw material route, the consumption of raw materials of each ton of products is 1.150t, the average price of petroleum benzene is 6350 yuan per ton, and the cost of the raw materials of each ton of products is 7303 yuan; the raw material cost of the technically improved ton product is reduced by 2579 yuan.
The invention is not limited to the specific technical solutions described in the above embodiments, and all technical solutions formed by equivalent substitutions are within the scope of the invention.
Claims (4)
1. A process for preparing maleic anhydride by n-butane oxidation is characterized by comprising the following steps:
TMP steam and n-butane steam are mixed and then enter an air-hydrocarbon mixer together with air to be mixed, the mixed gas enters a fixed bed reactor filled with a catalyst, and the reacted gas is cooled and refined to obtain a maleic anhydride product; the catalyst takes diatomite as a carrier, the weight content of the carrier is 20-40%, and the general formula of active components of the catalyst is as follows: v 1.0PaMobOmWherein a is 0.8-1.5, b is 0.05-0.5, and m is the number of oxygen atoms required by the valence of each element;
the reacted gas enters a secondary gas cooler after passing through a primary gas cooler and then enters an air cooler for cooling, the temperature of the primary gas cooler is 180-220 ℃, the cooling temperature of the secondary gas cooler is provided by boiler steam, and the temperature is 145-165 ℃;
the specific process steps for producing maleic anhydride by oxidizing n-butane after modification are as follows:
(1) liquid n-butane in the n-butane storage tank enters an n-butane evaporator, and is sent to an n-butane superheater after being heated and vaporized to obtain n-butane steam;
(2) pumping TMP into a TMP evaporator by a pump, mixing TMP steam with nitrogen, and then feeding the mixed TMP steam into a normal butane pipeline to be mixed with the butane steam in the step (1) to obtain organic steam;
(3) the air pressurized by the fan and heated by the air heater enters an air-hydrocarbon mixer to be mixed with the organic steam in the step (2), the obtained mixed gas enters a fixed bed tubular reactor filled with the catalyst together, the reacted gas enters a secondary gas cooler after passing through a primary gas cooler and then enters a partial cooler for cooling, the cooled reactant enters a crude anhydride separator, the gas enters an absorption tower, and the liquid crude anhydride enters a crude anhydride tank; washing part of the anhydride entering the absorption tower with water, collecting the washed anhydride in an acid water tank, and finally refining the anhydride and the anhydride in a crude anhydride tank to obtain a maleic anhydride product;
The preparation of the catalyst comprises the following steps:
(1) dispersing 100-400 meshes of diatomite into a mixed solution of isobutanol, benzyl alcohol and molybdenum isooctanoate, and reacting at 90-130 ℃ and a pressure of-5-30 Kpa to form a suspension;
(2) adding vanadium pentoxide and concentrated phosphoric acid into the suspension, depositing the generated precipitate on diatomite, filtering, drying at 100-150 ℃ for 4-24 h, and roasting at 200-400 ℃ for 1-8 h to form a precursor;
(3) and granulating the precursor into 10-60 meshes, tabletting the precursor into a hollow cylinder by using graphite as a lubricant, and activating the hollow cylinder at 400-500 ℃ for 10-20 h to obtain the catalyst.
2. The process according to claim 1, characterized in that: the flow rate of n-butane steam is 0.09-0.10 kg/Tube/h.
3. The process according to claim 1, characterized in that: the air flow is 2.0-2.1 NCM/Tube/h; the mixed gas contains 0.5 to 3.0ppm by volume of TMP.
4. The process according to claim 1, characterized in that: the fixed bed reaction pressure is 60-99 kPa, the molten salt temperature is 405-415 ℃, and the hot spot temperature is 430-450 ℃.
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| CN112705233A (en) * | 2019-10-24 | 2021-04-27 | 中国石油化工股份有限公司 | Vanadium phosphorus oxygen catalyst and preparation method and application thereof |
| CN115487753A (en) * | 2021-06-18 | 2022-12-20 | 济南隆凯能源科技有限公司 | Method and device for preparing acid anhydride by partial oxidation of hydrocarbon with variable-concentration feed |
| CN116082281A (en) * | 2023-02-22 | 2023-05-09 | 彭西周 | Process for recovering maleic anhydride from maleic anhydride-containing gas |
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| US4352755A (en) * | 1979-11-20 | 1982-10-05 | Imperial Chemical Industries Limited | Production of maleic anhydride |
| US5011945A (en) * | 1987-08-31 | 1991-04-30 | Amoco Corporation | Continuous process for the production of maleic anhydride |
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