CN113149806A - Composite solvent for extracting, rectifying and purifying 2,4, 4-trimethyl-1-pentene and purification method - Google Patents
Composite solvent for extracting, rectifying and purifying 2,4, 4-trimethyl-1-pentene and purification method Download PDFInfo
- Publication number
- CN113149806A CN113149806A CN202110418173.5A CN202110418173A CN113149806A CN 113149806 A CN113149806 A CN 113149806A CN 202110418173 A CN202110418173 A CN 202110418173A CN 113149806 A CN113149806 A CN 113149806A
- Authority
- CN
- China
- Prior art keywords
- pentene
- trimethyl
- solvent
- extraction
- triethylene glycol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
- C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
- C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/40—Extractive distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a composite solvent for extracting, rectifying and purifying 2,4, 4-trimethyl-1-pentene, which comprises the following components by mass: 20-40% of sulfone solvent; 60-75% of a nitrogen-containing solvent; 0.1-5% of an auxiliary agent; the nitrogen-containing solvent is at least one selected from succinonitrile, N-dimethylacetamide, N-Dimethylformamide (DMF), N-methylpyrrolidone (NMP), aminoethylpiperazine and N-formylmorpholine; the sulfone solvent is at least one selected from sulfolane, 3-methyl sulfolane, di-n-propyl sulfone, dimethyl sulfone and 3-methyl sulfolane; the auxiliary agent is at least one selected from triethylene glycol monomethyl ether, triethylene glycol dimethyl ether, triethylene glycol monoethyl ether and triethylene glycol diethyl ether. The solvent is used for extracting, rectifying and purifying crude TMPE, TMPE and 2,4, 4-trimethyl-2-pentene are effectively separated, and the purity TMPE is prepared.
Description
Technical Field
The invention relates to a purification method of 2,4, 4-trimethyl-1-pentene, in particular to a composite solvent for extracting, rectifying and purifying the 2,4, 4-trimethyl-1-pentene and a purification method of the 2,4, 4-trimethyl-1-pentene.
Background
2,4, 4-Trimethyl-1-pentene (2,4,6-Trimethyl-1-pentene, TMPE) is an important chemical intermediate, and is widely used for producing isononyl alcohol/aldehyde, octylphenol, octyldiphenylamine and the like. TMPE can prepare isononanal and isononanol through hydroformylation reaction, and is an important raw material for synthesizing PVC plasticizer and refrigerator oil. The reaction of TMPE with phenol produces octylphenol, which can be used to produce nonionic surfactants, oil-soluble phenolic resins, rubber vulcanizing agents, printing inks, coatings, and formulated insulating varnishes, rust inhibitors, and the like. The heavy alkyl product generated by TMPE hydrogenation can be a high-quality solvent without aromatic hydrocarbon and odor, and can also be used as an additive of kerosene and aviation fuel.
Isobutene dimerization and tert-butyl alcohol dehydration dimerization to prepare diisobutylene, wherein the obtained diisobutylene is usually a mixture of TMEP and 2,4, 4-trimethyl-2-pentene, and the content of TMPE in the diisobutylene is usually below 85 percent.
Because TMPE and 2,4, 4-trimethyl-2-pentene have similar structures and the boiling point difference is within 3 ℃, the content of 2,4, 4-trimethyl-1-pentene in diisobutylene is difficult to further improve by the conventional rectification separation process.
The extraction and rectification is to add an extracting agent or a solvent into raw material liquid so as to change the relative volatility of the original components and realize the separation of the components. Typically, the boiling point of the extractant is significantly higher than the boiling point of the components in the feed solution and does not form an azeotrope with the components. Extractive distillation is commonly used to separate solutions in which the components differ only slightly in boiling point (volatility). Although extractive distillation is widely applied to separation of butane and butene, butene and butadiene, diisopropylbenzene isomer, benzene and cyclohexane and other mixtures, the application report of the extractive distillation in separation of diisobutylene isomer is not seen at all.
Disclosure of Invention
In order to solve the problem of insufficient purity of 2,4, 4-trimethyl-1-pentene, the invention provides a solvent for separating 2,4, 4-trimethyl-1-pentene (TMPE) by extractive distillation and a use method thereof, the solvent is used for extracting, rectifying and purifying crude TMPE, TMPE and 2,4, 4-trimethyl-2-pentene are effectively separated, and the pure TMPE is prepared.
In order to achieve the above object, the present invention adopts the following technical solutions.
The invention provides a composite solvent for extracting, rectifying and purifying 2,4, 4-trimethyl-1-pentene, which comprises the following components by mass:
20-40% of sulfone solvent; 60-75% of a nitrogen-containing solvent; 0.1-5% of an auxiliary agent;
the nitrogen-containing solvent is at least one selected from succinonitrile, N-dimethylacetamide, N-Dimethylformamide (DMF), N-methylpyrrolidone (NMP), aminoethylpiperazine and N-formylmorpholine;
the sulfone solvent is at least one selected from sulfolane, 3-methyl sulfolane, di-n-propyl sulfone, dimethyl sulfone and 3-methyl sulfolane;
the auxiliary agent is at least one selected from triethylene glycol monomethyl ether, triethylene glycol dimethyl ether, triethylene glycol monoethyl ether and triethylene glycol diethyl ether.
Preferably, the complex solvent comprises the following components: 28-38% of a sulfone solvent; 60-70% of a nitrogen-containing solvent; 2-3% of an auxiliary agent.
Preferably, the nitrogen-containing solvent is one or two of N, N-dimethylformamide and N-methylpyrrolidone which are optionally mixed.
Preferably, the nitrogen-containing solvent consists of N, N-dimethylformamide and N-methylpyrrolidone, and the mass ratio of the NN-dimethylformamide to the N-methylpyrrolidone is 1: 4-9.
Preferably, the sulfone solvent is one or two of sulfolane and 3-methyl sulfolane optionally mixed.
Preferably, the auxiliary agent is at least one selected from the group consisting of triethylene glycol monomethyl ether and triethylene glycol dimethyl ether.
The invention provides a method for purifying 2,4, 4-trimethyl-1-pentene, which comprises the following steps of;
introducing the crude 2,4, 4-trimethyl-1-pentene into the middle part of an extractive distillation tower, introducing the composite solvent into the upper part of the extractive distillation tower, and discharging the 2,4, 4-trimethyl-1-pentene from the top of the extractive distillation tower after extractive distillation; after the 2,4, 4-trimethyl-2-pentene and the composite solvent are discharged from the bottom of the extractive distillation tower, the composite solvent is recovered by rectification separation and returned to the extractive distillation tower for recycling.
Preferably, the mass ratio of the composite solvent entering the extractive distillation tower to the crude 2,4, 4-trimethyl-1-pentene is 2-7:1, and the theoretical plate number of the extractive distillation tower is 20-80; the pressure at the top of the extraction and rectification tower is 60-220 kPa, and the temperature at the bottom of the extraction and rectification tower is 130-230 ℃.
Preferably, the mass ratio of the composite solvent entering the extractive distillation tower to the crude 2,4, 4-trimethyl-1-pentene is 2.5-5.5:1, and the theoretical plate number of the extractive distillation tower is 30-65; the pressure at the top of the extraction and rectification tower is 80-180 kPa, and the temperature at the bottom of the extraction and rectification tower is 140-185 ℃.
Preferably, the mass content of the 2,4, 4-trimethyl-1-pentene in the crude 2,4, 4-trimethyl-1-pentene is 76-85%; the mass content of the 2,4, 4-trimethyl-2-pentene is 15-24%.
The composite solvent for extracting, rectifying and purifying the 2,4, 4-trimethyl-1-pentene is used for purifying the 2,4, 4-trimethyl-1-pentene, and can effectively separate the 2,4, 4-trimethyl-1-pentene and the 2,4, 4-trimethyl-2-pentene, so that the purity of the 2,4, 4-trimethyl-1-pentene is over 88 percent.
The composite solvent provided by the invention, the sulfone solvent, the nitrogen-containing solvent and the auxiliary agent have synergistic effect, so that the solubility of the diisobutylene isomer is increased, the gas-liquid mass transfer performance is improved, the relative volatility of the diisobutylene component is improved, and the selectivity of the composite solvent to 2,4, 4-trimethyl-2-pentene is improved. The composite solvent has the advantages of high boiling point, stable property, good solubility to raw materials, high efficiency of extractive distillation on the basis of ensuring high selectivity, and capability of effectively separating 2,4, 4-trimethyl-1-pentene and 2,4, 4-trimethyl-2-pentene.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a composite solvent for purifying 2,4, 4-trimethyl-1-pentene by extractive distillation, which increases the solubility of diisobutylene isomer, improves the gas-liquid mass transfer performance, improves the selectivity of the composite solvent to 2,4, 4-trimethyl-2-pentene, has high efficiency of extractive distillation on the basis of ensuring high selectivity, and can effectively separate 2,4, 4-trimethyl-1-pentene and 2,4, 4-trimethyl-2-pentene.
On the basis of mass content, the composite solvent comprises the following components:
20-40% of sulfone solvent; 60-75% of a nitrogen-containing solvent; 0.1-5% of an auxiliary agent;
the nitrogen-containing solvent is at least one selected from succinonitrile, N-dimethylacetamide, N-dimethylformamide, N-methylpyrrolidone, aminoethylpiperazine and N-formylmorpholine;
the sulfone solvent is at least one selected from sulfolane, 3-methyl sulfolane, di-n-propyl sulfone, dimethyl sulfone and 3-methyl sulfolane;
the auxiliary agent is at least one selected from triethylene glycol monomethyl ether, triethylene glycol dimethyl ether, triethylene glycol monoethyl ether and triethylene glycol diethyl ether.
According to the present invention, preferably, the complex solvent comprises the following components: 28-38% of a sulfone solvent; 60-70% of a nitrogen-containing solvent; 2-3% of an auxiliary agent; on the basis of ensuring high selectivity, the composite solvent has higher efficiency of extractive distillation.
According to the invention, preferably, the nitrogen-containing solvent is one or two of N, N-dimethylformamide and N-methylpyrrolidone which are optionally mixed.
According to the invention, preferably, the nitrogen-containing solvent consists of N, N-dimethylformamide and N-methylpyrrolidone, and the mass ratio of the N, N-dimethylformamide to the N-methylpyrrolidone is 1: 4-9; the foregoing nitrogen-containing solvent increases the solubility of the diisobutylene isomer.
According to the invention, preferably, the sulfone solvent is one or two of sulfolane and 3-methyl sulfolane optionally mixed; the aforementioned sulfones further increase the solubility for the diisobutylene isomer.
According to the present invention, preferably, the auxiliary agent is selected from at least one of triethylene glycol monomethyl ether and triethylene glycol dimethyl ether.
The invention provides a method for purifying 2,4, 4-trimethyl-1-pentene, which comprises the following steps of;
introducing crude 2,4, 4-trimethyl-1-pentene into the middle part of an extraction rectifying tower, introducing the composite solvent into the upper part of the extraction rectifying tower, performing extraction rectification, discharging the 2,4, 4-trimethyl-1-pentene from the top of the extraction rectifying tower, returning one part of the 2,4, 4-trimethyl-1-pentene serving as tower top reflux to the extraction rectifying tower, and discharging the other part of the 2,4, 4-trimethyl-1-pentene out of a system; after the 2,4, 4-trimethyl-2-pentene and the composite solvent are discharged from the bottom of the extractive distillation tower, the composite solvent is recovered by rectification separation and returned to the extractive distillation tower for recycling.
According to the invention, preferably, the mass ratio of the composite solvent entering the extractive distillation tower to the crude 2,4, 4-trimethyl-1-pentene is 2-7:1, and the theoretical plate number of the extractive distillation tower is 20-80; the pressure at the top of the extraction and rectification tower is 60-220 kPa, and the temperature at the bottom of the extraction and rectification tower is 130-230 ℃; the process has high efficiency of extractive distillation, and can effectively separate 2,4, 4-trimethyl-1-pentene and 2,4, 4-trimethyl-2-pentene.
According to the invention, preferably, the mass ratio of the composite solvent entering the extractive distillation tower to the crude 2,4, 4-trimethyl-1-pentene is 2.5-5.5:1, and the theoretical plate number of the extractive distillation tower is 30-65; the pressure at the top of the extraction and rectification tower is 80-180 kPa, and the temperature at the bottom of the extraction and rectification tower is 140-185 ℃; by adopting the process conditions, the separation efficiency of the 2,4, 4-trimethyl-1-pentene is further improved, and the purity of the 2,4, 4-trimethyl-1-pentene is improved.
According to the invention, the mass content of the 2,4, 4-trimethyl-1-pentene in the crude 2,4, 4-trimethyl-1-pentene is preferably 76-85%; the mass content of the 2,4, 4-trimethyl-2-pentene is 15-24%.
In the present invention, unless otherwise specified, the content refers to mass content.
The present invention will be further described with reference to the following specific embodiments, specific examples, comparative examples and test results.
Example 1
Introducing a composite solvent (60% of N, N-dimethylformamide, 38% of sulfolane and 2% of triethylene glycol dimethyl ether) from the upper part of the extraction and rectification tower, introducing crude 2,4, 4-trimethyl-1-pentene (the purity is 84%) from the middle part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 50; the pressure at the top of the extraction and rectification tower is 120kPa, the temperature at the top of the extraction and rectification tower is 99 ℃, and the temperature at the bottom of the extraction and rectification tower is 140 ℃.
Example 2
The composite solvent is 8.45 percent of N, N-dimethylformamide, 56.55 percent of N-methylpyrrolidone, 32 percent of sulfolane and 3 percent of triethylene glycol dimethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 101 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
Example 3
The composite solvent is 65% of N, N-dimethylformamide, 32% of sulfolane and 3% of triethylene glycol dimethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 101 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
Example 4
The composite solvent is 65% of N-methyl pyrrolidone, 32% of sulfolane and 3% of triethylene glycol dimethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 101 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
Example 5
The composite solvent is 8.45 percent of N, N-dimethylformamide, 56.55 percent of N-methyl pyrrolidone, 32 percent of dimethyl sulfone and 3 percent of triethylene glycol dimethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 101 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
Example 6
The composite solvent is 8.45 percent of N, N-dimethylformamide, 56.55 percent of N-methylpyrrolidone, 32 percent of sulfolane and 3 percent of triethylene glycol diethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 101 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
Example 7
The composite solvent is 9.75 percent of N, N-dimethylformamide, 65.25 percent of N-methyl pyrrolidone, 24 percent of sulfolane and 1 percent of triethylene glycol dimethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 101 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
Example 8
The composite solvent is 65% of nitrogen-containing solvent (the mass ratio of succinonitrile to N-methyl pyrrolidone is 1:5), 32% of sulfolane and 3% of triethylene glycol dimethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 101 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
Example 9
The composite solvent is 8.45 percent of N, N-dimethylformamide, 56.55 percent of N-methylpyrrolidone, 32 percent of sulfolane and 3 percent of triethylene glycol dimethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 6: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 100 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
Example 10
The composite solvent is 8.45 percent of N, N-dimethylformamide, 56.55 percent of N-methylpyrrolidone, 32 percent of sulfolane and 3 percent of triethylene glycol dimethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 25; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 102 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
Example 11
The composite solvent is 8.45 percent of N, N-dimethylformamide, 56.55 percent of N-methylpyrrolidone, 32 percent of sulfolane and 3 percent of triethylene glycol dimethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 102 ℃, and the temperature at the bottom of the extraction and rectification tower is 200 ℃.
Example 12
The difference from example 4 is that the composite solvent and the crude 2,4, 4-trimethyl-1-pentene (purity 84%) are introduced from the middle of the extractive distillation column; the remaining procedure was as in example 4.
Comparative example 1
The composite solvent is 8.45 percent of N, N-dimethylformamide, 56.55 percent of N-methylpyrrolidone and 35 percent of sulfolane; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 101 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
Comparative example 2
The composite solvent is 97% of sulfolane and 3% of triethylene glycol dimethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 101 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
Comparative example 3
The composite solvent is 84.4 percent of N-methyl pyrrolidone, 12.6 percent of N, N-dimethylformamide and 3 percent of triethylene glycol dimethyl ether; introducing crude 2,4, 4-trimethyl-1-pentene (with the purity of 84%) from the middle part of the extraction and rectification tower, introducing a composite solvent from the upper part of the extraction and rectification tower, wherein the mass ratio of the composite solvent to the crude 2,4, 4-trimethyl-1-pentene is 3: 1; the theoretical plate number of the extraction rectifying tower is 60; the pressure at the top of the extraction and rectification tower is 100kPa, the temperature at the top of the extraction and rectification tower is 101 ℃, and the temperature at the bottom of the extraction and rectification tower is 160 ℃.
TABLE 1 purity of purified 2,4, 4-trimethyl-1-pentene in examples 1-10 and comparative examples 1-3
| Examples | Composite solvent | Purity of TMPE |
| Example 1 | 60% of DMF, 38% of sulfolane and 2% of triethylene glycol dimethyl ether | 88％ |
| Example 2 | 56.55% NMP, 8.45% DMF, 32% sulfolane, 3% triethylene glycol dimethyl ether | 98.1％ |
| Example 3 | 65% of DMF, 32% of sulfolane and 3% of triethylene glycol dimethyl ether | 94.5％ |
| Example 4 | 65% of NMP, 32% of sulfolane and 3% of triethylene glycol dimethyl ether | 95.3％ |
| Example 5 | 56.55% NMP, 8.45% DMF, 32% dimethyl sulfone, 3% triethylene glycol dimethyl ether | 90.9％ |
| Example 6 | 56.55% NMP, 8.45% DMF, 32% sulfolane, 3% triethylene glycol diethyl ether | 90.2％ |
| Example 7 | 65.25% NMP, 9.75% DMF, 24% sulfolane, 1% triethylene glycol dimethyl ether | 94.1％ |
| Example 8 | 56.55% of NMP, 8.45% of succinonitrile, 32% of sulfolane and 3% of triethylene glycol dimethyl ether | 89.0％ |
| Example 9 | 56.55% NMP, 8.45% DMF, 32% sulfolane, 3% triethylene glycol dimethyl ether | 92.2％ |
| Example 10 | 56.55% NMP, 8.45% DMF, 32% sulfolane, 3% triethylene glycol dimethyl ether | 88.3％ |
| Example 11 | 56.55% of NMP, 8.45% of DMF, 32% of sulfolane, | 89.6％ |
| Example 12 | 65% of NMP, 32% of sulfolane and 3% of triethylene glycol dimethyl ether | 90.7％ |
| Comparative example 1 | 56.55% NMP, 8.45% DMF, 35% sulfolane | 85.2％ |
| Comparative example 2 | 97% sulfolane, 3% triethylene glycol dimethyl ether | 86.0％ |
| Comparative example 3 | 84.4 percent of NMP, 12.6 percent of DMF, and 3 percent of triethylene glycol dimethyl ether | 85.1％ |
The results in table 1 show that the solvent described in the present application can effectively separate 2,4, 4-trimethyl-1-pentene and 2,4, 4-trimethyl-2-pentene, and the purity of the purified 2,4, 4-trimethyl-1-pentene is up to 88% or more, and up to 98.1%, which significantly improves the purity of 2,4, 4-trimethyl-1-pentene.
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, numerous simple modifications can be made to the technical solution of the invention, including combinations of the specific features in any suitable way, and the invention will not be further described in relation to the various possible combinations in order to avoid unnecessary repetition. Such simple modifications and combinations should be considered within the scope of the present disclosure as well.
Claims (10)
1. The composite solvent for extracting, rectifying and purifying the 2,4, 4-trimethyl-1-pentene is characterized by comprising the following components in percentage by mass:
20-40% of sulfone solvent;
60-75% of a nitrogen-containing solvent;
0.1-5% of an auxiliary agent;
the nitrogen-containing solvent is at least one selected from succinonitrile, N-dimethylacetamide, N-dimethylformamide, N-methylpyrrolidone, aminoethylpiperazine and N-formylmorpholine;
the sulfone solvent is at least one selected from sulfolane, 3-methyl sulfolane, di-n-propyl sulfone, dimethyl sulfone and 3-methyl sulfolane;
the auxiliary agent is at least one selected from triethylene glycol monomethyl ether, triethylene glycol dimethyl ether, triethylene glycol monoethyl ether and triethylene glycol diethyl ether.
2. The composite solvent according to claim 1, wherein the composite solvent comprises the following components: 28-38% of a sulfone solvent;
60-70% of a nitrogen-containing solvent;
2-3% of an auxiliary agent.
3. The composite solvent according to claim 1 or 2, wherein the nitrogen-containing solvent is one or two of N, N-dimethylformamide and N-methylpyrrolidone.
4. The composite solvent according to claim 3, wherein the nitrogen-containing solvent consists of N, N-dimethylformamide and N-methylpyrrolidone; preferably, the mass ratio of the NN-dimethylformamide to the N-methylpyrrolidone is 1: 4-9.
5. The composite solvent according to claim 1 or 2, wherein the sulfone solvent is one or two of sulfolane and 3-methyl sulfolane.
6. The composite solvent according to claim 1 or 2, wherein the auxiliary agent is at least one selected from triethylene glycol monomethyl ether and triethylene glycol dimethyl ether.
7. A process for purifying 2,4, 4-trimethyl-1-pentene, comprising; introducing crude 2,4, 4-trimethyl-1-pentene into the middle part of an extractive distillation tower, introducing the composite solvent as defined in any one of claims 1 to 6 into the upper part of the extractive distillation tower, and discharging the 2,4, 4-trimethyl-1-pentene from the top of the extractive distillation tower after extractive distillation; after the 2,4, 4-trimethyl-2-pentene and the composite solvent are discharged from the bottom of the extractive distillation tower, the composite solvent is recovered by rectification separation and returned to the extractive distillation tower for recycling.
8. The purification method according to claim 7, wherein the mass ratio of the composite solvent entering the extractive distillation column to the crude 2,4, 4-trimethyl-1-pentene is 2-7:1, and the number of theoretical plates of the extractive distillation column is 20-80; the pressure at the top of the extraction and rectification tower is 60-220 kPa, and the temperature at the bottom of the extraction and rectification tower is 130-230 ℃.
9. The purification method according to claim 7 or 8, wherein the mass ratio of the composite solvent entering the extractive distillation column to the crude 2,4, 4-trimethyl-1-pentene is 2.5-5.5:1, and the number of theoretical plates of the extractive distillation column is 30-65; the pressure at the top of the extraction and rectification tower is 80-180 kPa, and the temperature at the bottom of the extraction and rectification tower is 140-185 ℃.
10. The purification method according to claim 7 or 8, wherein the crude 2,4, 4-trimethyl-1-pentene contains 76 to 85% by mass of 2,4, 4-trimethyl-1-pentene and 15 to 24% by mass of 2,4, 4-trimethyl-2-pentene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110418173.5A CN113149806A (en) | 2021-04-19 | 2021-04-19 | Composite solvent for extracting, rectifying and purifying 2,4, 4-trimethyl-1-pentene and purification method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110418173.5A CN113149806A (en) | 2021-04-19 | 2021-04-19 | Composite solvent for extracting, rectifying and purifying 2,4, 4-trimethyl-1-pentene and purification method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113149806A true CN113149806A (en) | 2021-07-23 |
Family
ID=76868572
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110418173.5A Pending CN113149806A (en) | 2021-04-19 | 2021-04-19 | Composite solvent for extracting, rectifying and purifying 2,4, 4-trimethyl-1-pentene and purification method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113149806A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1108232A (en) * | 1993-12-06 | 1995-09-13 | 戈里特斯奇公司 | Process to recover benzene from mixed hydrocarbons |
| CN1900032A (en) * | 2006-07-06 | 2007-01-24 | 湖南长岭石化科技开发有限公司 | Method for producing benzene aromatic hydrocarbon from crude benzole |
| CN109867583A (en) * | 2019-03-15 | 2019-06-11 | 丹东明珠特种树脂有限公司 | 2,4,4- trimethyl -1- amylene process and its system and device are obtained by four heat bodied oil of carbon |
-
2021
- 2021-04-19 CN CN202110418173.5A patent/CN113149806A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1108232A (en) * | 1993-12-06 | 1995-09-13 | 戈里特斯奇公司 | Process to recover benzene from mixed hydrocarbons |
| CN1900032A (en) * | 2006-07-06 | 2007-01-24 | 湖南长岭石化科技开发有限公司 | Method for producing benzene aromatic hydrocarbon from crude benzole |
| CN109867583A (en) * | 2019-03-15 | 2019-06-11 | 丹东明珠特种树脂有限公司 | 2,4,4- trimethyl -1- amylene process and its system and device are obtained by four heat bodied oil of carbon |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11731922B2 (en) | Method for separating aromatic hydrocarbon using extractive distillation | |
| KR101700986B1 (en) | Fractional extraction of butadiene | |
| CN104030876A (en) | System and method for preparation of isobutane through combined extractive distillation and hydrogenation | |
| CN103160310A (en) | Composite solvent and extraction method for extracting and separating aromatic hydrocarbons | |
| CN112135809A (en) | Method for producing fuel additive using hydration unit | |
| CN112745907B (en) | Method for removing oxygen-containing compounds in Fischer-Tropsch synthetic oil | |
| CN108929188B (en) | From mixing C4Method for separating butane and butylene by extractive distillation in hydrocarbon raw material | |
| CN104703951B (en) | Butadiene extracts pre-absorption tower | |
| CN105602613B (en) | The method of phenol, aromatic hydrocarbons and alkane in one-step method separation coal direct liquefaction oil | |
| CN101468938B (en) | Composite solvent for extracting, distilling and separating styrene in hydrocarbons mixture, and method therefor | |
| CN113149806A (en) | Composite solvent for extracting, rectifying and purifying 2,4, 4-trimethyl-1-pentene and purification method | |
| CN112745913B (en) | Method for removing oxygen-containing compounds in Fischer-Tropsch synthetic oil | |
| CN102276430A (en) | Separation of glycol mono-tertiary-butyl ether and glycol di-tertiary-butyl ether | |
| JP2842091B2 (en) | Method for obtaining high-purity 1-butene and 2-butene | |
| DE3339157A1 (en) | METHOD FOR OBTAINING A CONJUGATED DIOLEFIN AND / OR OLEFIN FROM A C (DOWN ARROW) 4 (DOWN ARROW) - OR C (DOWN ARROW) 5 (DOWN ARROW) HYDROCARBON MIXTURE | |
| US4421607A (en) | Process for extractive distillation of plural hydrocarbon mixtures | |
| CN102249837A (en) | Purification method for butylene by chemical separation process | |
| WO2024060399A1 (en) | Separation method for high-temperature fischer-tropsch synthesized light oil | |
| CN112745908B (en) | Method for removing oxygen-containing compounds in Fischer-Tropsch synthesis light oil | |
| CN108997077B (en) | Composite solvent and method for extracting, rectifying and separating aromatic hydrocarbon from hydrocarbon mixture | |
| CN106083516B (en) | The method that 1,3- butadiene in alkylate oil raw materials for production is removed using extracting rectifying | |
| CN117946729A (en) | Composite solvent for aromatic hydrocarbon extraction and method for extracting aromatic hydrocarbon | |
| CN115806464A (en) | Process for separating 1-hexene, 1-heptene and 1-octene from a hydrocarbon-containing stream | |
| CN106478356B (en) | Method for separating pentene-1 and pentene-2 from carbon five byproduct fraction | |
| CN116003206A (en) | Method for extracting styrene by cracking carbon eight |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |