CN109748781B - Method for treating high-sulfur-carbon four-raw material and co-producing low-sulfur MTBE product - Google Patents
Method for treating high-sulfur-carbon four-raw material and co-producing low-sulfur MTBE product Download PDFInfo
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Abstract
The invention discloses a method for treating high-sulfur-carbon four-raw materials and co-producing low-sulfur MTBE products, which comprises the following steps: (1) conveying the high-sulfur and high-carbon four-raw material into an MTBE (methyl tert-butyl ether) catalytic distillation tower, supplementing a proper amount of methanol above a feed inlet, and extracting an azeotrope of carbon four-hydrocarbon and methanol from the top of the MTBE catalytic distillation tower; (2) sending the azeotrope of the carbon-four hydrocarbons and the methanol extracted from the top of the MTBE catalytic rectifying tower to a water scrubber to remove the methanol, and separating to obtain a low-sulfur carbon-four raw material; (3) and (3) sending the high-sulfur MTBE product extracted from the tower kettle of the MTBE catalytic distillation tower into an MTBE refining tower for rectification treatment, extracting the low-sulfur MTBE product from the tower top, and removing heavy-component sulfides from the tower kettle. The sulfur content of the low-sulfur carbon four-raw material obtained after desulfurization treatment by the method is less than 5ppm, and the low-sulfur carbon four-raw material can be used as a high-quality carbon four-raw material for carbon four-deep processing technologies such as isooctane and butene isomerization. Meanwhile, the sulfur content of the low-sulfur MTBE product obtained after refining is less than 10ppm, and the product yield can reach 90-98%.
Description
Technical Field
The invention relates to the technical field of refining of carbon four raw materials, in particular to a method for treating a high-sulfur carbon four raw material and co-producing a low-sulfur MTBE product.
Background
MTBE (methyl tert-butyl ether) is English abbreviation of methyl tert-butyl ether, formula C5H12O, structural formula CH3-O-C(CH3)3And the boiling point is 55.2 ℃, and the liquid is colorless, transparent and high-octane-value liquid and has ether-like smell. MTBE is used in small amount in chemical industry, mainly as an ideal blending component of clean gasoline with high octane number, and has been widely used as a gasoline additive all over the world.
In recent years, the quality standard of domestic motor gasoline is rapidly upgraded, the limit value of sulfur content is greatly reduced, and the national V emission standard requires that the mass fraction of sulfur in gasoline is not more than 10 mg/kg. If the MTBE product is used as a gasoline high-octane value blending component and the sulfur content of the MTBE product is too high, the risk that the sulfur content of the gasoline exceeds the standard is increased greatly.
MTBE is mainly formed by the addition reaction of methanol and isobutene, and low-cost mixed C-C hydrocarbons are frequently used as reaction raw materials in the industry at present. The sulfur content of the methanol is generally lower than 5ppm, while the mixed C-C raw material is often carried with a certain amount of sulfides, in the MTBE production process, the MTBE and the residual C-C and methanol in the reaction are separated in a catalytic rectifying tower, an azeotrope of the C-C and methanol is extracted from the tower top, the residual C-C four components are separated and discharged after the methanol is removed by washing, and the methanol is recycled.
The reduction of the sulfur content of the MTBE product can be achieved by reducing the sulfur content of the feed carbon four or by rectifying the MTBE product. At present, the process of removing mercaptan from liquefied gas in refineries in China mainly adopts a Merox agent alkali extraction-liquid phase catalytic oxidation mercaptan removal process. In an extraction tower, mercaptan in the liquefied gas reacts with an alkaline solution (sulfonated cobalt phthalocyanine alkaline solution) to generate sodium mercaptan and the sodium mercaptan is transferred to an alkaline phase; the agent alkali liquor separated from the liquefied gas enters an oxidation regeneration tower, sodium mercaptan in the alkali liquor is oxidized into disulfide under the action of air, mercaptan removal is realized, and meanwhile, the alkali liquor and the catalyst are regenerated and recycled. The patent CN1632072A adopts a mode of combining liquid-liquid agent alkali extraction and fixed bed catalytic oxidation regeneration technology, thereby improving the mercaptan extraction efficiency and the alkali liquor regeneration efficiency; in patent CN101474574A, the desulfurization depth and efficiency are improved by adopting the processes of performing function enhancement on a circulating solvent, three-phase mixing and enhancing regeneration, separating a regenerated catalyst from an extraction agent, deoxidizing the circulating agent and the like. However, in the process of liquefied gas desulfurization, when the alkali liquor containing the catalyst is subjected to mercaptan extraction, part of sodium mercaptan is inevitably generated into disulfide which is carried into a refined liquefied gas product, so that the total sulfur removal effect is reduced, and the outgoing liquefied gas can not meet the requirement of the total sulfur content. For downstream carbon four deep processing enterprises receiving liquefied gas, carbon four raw materials with over-high sulfur content can generate corrosion and accelerated corrosion effects on metals under certain conditions, and easily deactivate catalysts of downstream deep processing devices. If the low-sulfur MTBE product is produced by deep desulfurization of the raw material carbon four directly, the sulfur content of the raw material carbon four needs to be controlled below 2ppm in order to meet the existing sulfur content standard, so that the precise desulfurization standard is realized, high cost is needed, and great challenges are brought to the difficulty. In contrast, the sulfur content of the MTBE product reaches the standard by adopting a rectification mode of the MTBE product, which is usually realized by only adding a few devices such as a rectification tower on the existing MTBE production device, and patents CN102491882A and the like introduce a method for obtaining the MTBE product with lower sulfur content by re-rectifying the sulfur-containing MTBE.
Disclosure of Invention
The invention aims to solve the technical problems that the existing raw material carbon four-sulfur is high in content, difficult to process and high in cost, and provides a method for processing a high-sulfur carbon four-raw material and co-producing a low-sulfur MTBE product.
A method of processing a high sulfur carbon four feedstock in combination with producing a low sulfur MTBE product, comprising the steps of:
(1) sending the high-sulfur carbon four raw material into an MTBE catalytic rectifying tower, supplementing a proper amount of methanol above a feed inlet, and extracting an azeotrope of carbon four hydrocarbons and methanol from the top of the MTBE catalytic rectifying tower; because the boiling point of most sulfides contained in the raw material of carbon four is higher than that of hydrocarbon of carbon four, the sulfides can be enriched in the tower kettle of the catalytic rectifying tower and can be extracted along with the MTBE product;
(2) sending the azeotrope of the carbon-four hydrocarbons and the methanol extracted from the top of the MTBE catalytic rectifying tower to a water scrubber to remove the methanol, and separating to obtain a low-sulfur carbon-four raw material; the sulfur content is less than 5 ppm;
(3) and (3) sending the high-sulfur MTBE product extracted from the tower kettle of the MTBE catalytic distillation tower into an MTBE refining tower for rectification treatment, extracting the low-sulfur MTBE product from the tower top, and removing heavy-component sulfides from the tower kettle.
Preferably, in the step (1), the sulfur content of the high sulfur carbon four raw material is 50-500ppm, and the mass concentration of isobutene is 0-50%.
Preferably, in the step (1), the operating conditions of the MTBE catalytic distillation tower are as follows: the temperature of the tower bottom is 120 ℃ and 140 ℃, the temperature of the tower top is 45-75 ℃, and the pressure of the tower top is 0.3-0.8 MPa.
Preferably, the operating conditions of the MTBE purification column in step (3): the temperature of the tower bottom is 120 ℃ and 140 ℃, the temperature of the top of the tower is 50-70 ℃, and the pressure of the top of the tower is 0-0.3 MPa.
Preferably, the mass concentration of isobutene in the feed of the MTBE catalytic distillation tower is controlled to be 0-5.0% in the step (1).
Preferably, the low sulfur MTBE product described in step (3) has less than 10ppm sulfur.
The sulfur content of the low-sulfur carbon four-raw material obtained after desulfurization treatment by the method is less than 5ppm, and the low-sulfur carbon four-raw material can be used as a high-quality carbon four-raw material for carbon four-deep processing technologies such as isooctane and butene isomerization. Meanwhile, the sulfur content of the low-sulfur MTBE product obtained after refining is less than 10ppm, and the product yield can reach 90-98%.
Drawings
FIG. 1 is a flow chart of the treatment method of the present invention.
Description of drawings: 1. etherification reaction materials, 2 high sulfur carbon four raw materials, 3 methanol feeding, 4, an MTBE catalytic distillation tower, 5, a water washing tower, 6, water replenishing of the water washing tower, 7, low sulfur carbon four raw materials, 8, water outlet of the water washing tower, 9, an MTBE refining tower, 10, low sulfur MTBE products, 11, heavy component sulfide
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, but the technical solutions do not limit the scope of the present invention.
Referring to fig. 1, the method for treating the high sulfur-carbon-four raw material and co-producing the low-sulfur MTBE product comprises the step of feeding the high sulfur-carbon-four raw material and the material from an etherification reactor into an MTBE catalytic rectifying tower, wherein the sulfur content of the high sulfur-carbon-four raw material is 50-500ppm, and the mass concentration of isobutene is 0-50%. The mass concentration of isobutene in the feed of the MTBE catalytic rectifying tower is controlled to be 0-5.0% by adjusting the feed amount of the high-sulfur-carbon four-raw material and the material amount discharged from the etherification reactor. The MTBE catalytic rectification tower comprises a rectification section, a catalytic reaction section and a stripping section, wherein a reaction catalyst and a filler are filled in the catalytic reaction section, the rectification section is a filler, and the stripping section is a tower plate. The lower part of the catalytic reaction section comprises one or more high-sulfur carbon four feeding holes and a methanol feeding hole, and the methanol feeding hole is positioned above the high-sulfur carbon four feeding holes. And supplementing a proper amount of methanol raw material into the catalytic rectifying tower at a methanol supplementing feed inlet, carrying out catalytic reaction on isobutene in the carbon four raw material and methanol in a catalytic rectifying reaction section to generate an MTBE product, collecting an azeotrope formed by the residual carbon four components and the methanol from the top of the tower, washing the azeotrope in a washing tower to remove the methanol, and collecting the low-sulfur carbon four raw material from the top of the washing tower. And sulfide in the raw material of the carbon IV falls into a tower kettle of the MTBE catalytic rectification tower due to high boiling point in the separation process, is extracted along with an MTBE product, then the high-sulfur MTBE product extracted from the tower kettle of the MTBE catalytic rectification tower is sent into an MTBE refining tower for refining and separation, the low-sulfur MTBE product is extracted from the tower top of the MTBE refining tower, and heavy-component sulfide is removed from the tower kettle.
Wherein, the operation conditions of the catalytic distillation tower are as follows: the temperature of the tower bottom is 120-140 ℃, the temperature of the tower top is 45-75 ℃, the pressure of the tower top is 0.3-0.8MPa, and the sulfur content of the tower bottom is 200-800 ppm.
Operating conditions of the MTBE refining tower: the temperature of the tower bottom is 120 ℃ and 140 ℃, the temperature of the top of the tower is 50-70 ℃, and the pressure of the top of the tower is 0-0.3 MPa.
The sulfur content of the low-sulfur carbon four raw material obtained by the desulfurization treatment is less than 5ppm, and the low-sulfur carbon four raw material can be used as a high-quality carbon four raw material for a carbon four deep processing technology such as isooctane and butene isomerization. The sulfur content of the low-sulfur MTBE product obtained after refining is less than 10ppm, and the product yield can reach 90-98%.
Specific examples of the invention are shown in Table 1 below
TABLE 1
Specifically, the method comprises the following steps:
example 1
Feeding a four-carbon raw material with 50ppm of sulfur content and 4.5% of isobutene content and materials of an etherification reactor into an MTBE (methyl tert-butyl ether) catalytic rectification tower, and controlling the mass concentration of isobutene in the feed of the MTBE catalytic rectification tower to be 0-5.0%, the temperature of a tower kettle to be 125 ℃, the temperature of a tower top to be 53 ℃, the pressure of the tower top to be 0.41MPa and the content of the four-carbon sulfur extracted from the tower top to be 1.1ppm by adjusting the feed amount of the four-carbon raw material with high sulfur content and the amount of the materials discharged from the etherification reactor; then the MTBE with the sulfur content of 215ppm in the tower bottom is sent into an MTBE refining tower, the temperature of the tower bottom of the refining tower is 124 ℃, the temperature of the tower top is 56 ℃, the pressure of the tower top is 0.15MPa, the sulfur content of the MTBE product extracted from the tower top is 2.1ppm, and the yield is 98%.
Example 2
Feeding a carbon four raw material with the sulfur content of 493ppm and the isobutene content of 3.8% and materials of an etherification reactor into an MTBE (methyl tert-butyl ether) catalytic rectifying tower, and controlling the mass concentration of isobutene in the feed of the MTBE catalytic rectifying tower to be 0-5.0%, the temperature of a tower kettle to be 123 ℃, the temperature of a tower top to be 51 ℃, the pressure of the tower top to be 0.40MPa and the content of carbon four sulfur extracted from the tower top to be 3.6ppm by adjusting the feed amount of the high-sulfur carbon four raw material and the amount of the materials discharged from the etherification reactor; and then delivering the MTBE with the sulfur content of 790ppm in the tower bottom into an MTBE refining tower, wherein the tower bottom temperature of the refining tower is 134 ℃, the tower top temperature is 61 ℃, the tower top pressure is 0.21MPa, the sulfur content of the MTBE product extracted from the tower top is 6.2ppm, and the yield is 94%.
Example 3
Feeding a C-four raw material with 195ppm of sulfur content and 6.1% of isobutene content and materials of an etherification reactor into an MTBE (methyl tert-butyl ether) catalytic rectifying tower, and controlling the mass concentration of isobutene in the feed of the MTBE catalytic rectifying tower to be 0-5.0%, the temperature of a tower kettle to be 127 ℃, the temperature of a tower top to be 54 ℃, the pressure of the tower top to be 0.43MPa and the content of C-S extracted from the tower top to be 2.2ppm by adjusting the feed amount of the C-four raw material with high sulfur content and the amount of the materials discharged from the etherification reactor; and then delivering the MTBE with the sulfur content of 396ppm in the tower bottom into an MTBE refining tower, wherein the tower bottom temperature of the refining tower is 128 ℃, the tower top temperature is 57 ℃, the tower top pressure is 0.16MPa, the sulfur content of the MTBE product extracted from the tower top is 4.1ppm, and the yield is 96%.
Example 4
Feeding a four-carbon raw material with 415ppm of sulfur content and 14.2% of isobutene content and materials of an etherification reactor into an MTBE (methyl tert-butyl ether) catalytic rectification tower, and controlling the mass concentration of isobutene in the feed of the MTBE catalytic rectification tower to be 0-5.0%, the temperature of a tower kettle to be 128 ℃, the temperature of a tower top to be 57 ℃, the pressure of the tower top to be 0.48MPa and the content of the four-carbon sulfur extracted from the tower top to be 2.3ppm by adjusting the feed amount of the four-carbon raw material with high sulfur content and the amount of the materials discharged from the etherification reactor; and then delivering the MTBE with the sulfur content of 515ppm in the tower bottom into an MTBE refining tower, wherein the tower bottom temperature of the refining tower is 129 ℃, the tower top temperature is 57 ℃, the tower top pressure is 0.16MPa, the sulfur content of the MTBE product extracted from the tower top is 4.6ppm, and the yield is 95%.
Example 5
Feeding a carbon four raw material with 320ppm of sulfur content and 0.05 percent of isobutene content and materials of an etherification reactor into an MTBE (methyl tert-butyl ether) catalytic rectification tower, and controlling the mass concentration of isobutene in the feed of the MTBE catalytic rectification tower to be 0-5.0 percent, the temperature of a tower kettle to be 122 ℃, the temperature of a tower top to be 51 ℃, the pressure of the tower top to be 0.40MPa and the content of the carbon four sulphur extracted from the tower top to be 3.1ppm by adjusting the feed amount of the high-sulfur carbon four raw material and the amount of the materials discharged from the etherification reactor; and then delivering the MTBE with the sulfur content in the tower kettle of 671ppm into an MTBE refining tower, wherein the tower kettle temperature of the refining tower is 126 ℃, the tower top temperature is 56 ℃, the tower top pressure is 0.15MPa, the sulfur content of the MTBE product extracted from the tower top is 5.3ppm, and the yield is 95%.
Example 6
Feeding a four-carbon raw material with 174ppm of sulfur content and 25.4% of isobutene content and materials of an etherification reactor into an MTBE (methyl tert-butyl ether) catalytic rectification tower, and controlling the mass concentration of isobutene in the feed of the MTBE catalytic rectification tower to be 0-5.0%, the temperature of a tower kettle to be 133 ℃, the temperature of a tower top to be 58 ℃, the pressure of the tower top to be 0.51MPa and the content of the four-carbon sulphur extracted from the tower top to be 1.7ppm by adjusting the feed amount of the four-carbon raw material with high sulfur content and the amount of the materials discharged from the etherification reactor; then the MTBE with the sulfur content of 265ppm in the tower bottom is sent into an MTBE refining tower, the temperature of the tower bottom of the refining tower is 125 ℃, the temperature of the tower top is 56 ℃, the pressure of the tower top is 0.17MPa, the sulfur content of the MTBE product extracted from the tower top is 2.4ppm, and the yield is 97%.
Example 7
Feeding a four-carbon raw material with 224ppm of sulfur and 47.2 percent of isobutene and materials of an etherification reactor into an MTBE (methyl tert-butyl ether) catalytic rectifying tower, and controlling the mass concentration of isobutene in the feed of the MTBE catalytic rectifying tower to be 0-5.0 percent, the temperature of a tower kettle to be 124 ℃, the temperature of a tower top to be 54 ℃, the pressure of the tower top to be 0.45MPa and the content of the four-carbon sulfur extracted from the tower top to be 1.5ppm by adjusting the feed amount of the four-carbon raw material with high sulfur and the amount of the materials discharged from the etherification reactor; then the MTBE with the sulfur content of 270ppm in the tower bottom is sent into an MTBE refining tower, the temperature of the tower bottom of the refining tower is 128 ℃, the temperature of the tower top is 57 ℃, the pressure of the tower top is 0.18MPa, the sulfur content of the MTBE product extracted from the tower top is 2.3ppm, and the yield is 97%.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (4)
1. A method for treating high-sulfur-carbon four-raw materials and co-producing low-sulfur MTBE products is characterized by comprising the following steps:
(1) sending the high-sulfur carbon four raw material into an MTBE catalytic rectifying tower, supplementing a proper amount of methanol above a feed inlet, and extracting an azeotrope of carbon four hydrocarbons and methanol from the top of the MTBE catalytic rectifying tower;
(2) sending the azeotrope of the carbon-four hydrocarbons and the methanol extracted from the top of the MTBE catalytic rectifying tower to a water scrubber to remove the methanol, and separating to obtain a low-sulfur carbon-four raw material;
(3) conveying the high-sulfur MTBE product extracted from the tower kettle of the MTBE catalytic distillation tower into an MTBE refining tower for rectification treatment, extracting the low-sulfur MTBE product from the tower top, and removing heavy-component sulfides from the tower kettle;
the sulfur content of the high sulfur carbon four raw material in the step (1) is 50-500ppm, and the mass concentration of isobutene is 0-50%;
in the step (1), the mass concentration of isobutene in the feed of the MTBE catalytic distillation tower is controlled to be 0-5.0%.
2. The process of claim 1 for processing a high sulfur carbon four feedstock with co-production of low sulfur MTBE products, wherein: the operating conditions of the MTBE catalytic distillation tower in the step (1) are as follows: the temperature of the tower bottom is 120 ℃ and 140 ℃, the temperature of the tower top is 45-75 ℃, and the pressure of the tower top is 0.3-0.8 MPa.
3. The process of claim 1 for processing a high sulfur carbon four feedstock with co-production of low sulfur MTBE products, wherein: operating conditions of the MTBE refining tower in the step (3): the temperature of the tower bottom is 120 ℃ and 140 ℃, the temperature of the top of the tower is 50-70 ℃, and the pressure of the top of the tower is 0-0.3 MPa.
4. The process of claim 1 for processing a high sulfur carbon four feedstock with co-production of low sulfur MTBE products, wherein: the sulfur content of the low sulfur MTBE product in the step (3) is less than 10 ppm.
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