CN107266278B - High-purity production method of high-solubility aromatic hydrocarbon solvent GF-S1800 - Google Patents
High-purity production method of high-solubility aromatic hydrocarbon solvent GF-S1800 Download PDFInfo
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- CN107266278B CN107266278B CN201710595954.5A CN201710595954A CN107266278B CN 107266278 B CN107266278 B CN 107266278B CN 201710595954 A CN201710595954 A CN 201710595954A CN 107266278 B CN107266278 B CN 107266278B
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- 239000002904 solvent Substances 0.000 title claims abstract description 33
- 150000004945 aromatic hydrocarbons Chemical class 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 45
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 claims abstract description 30
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 18
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000008096 xylene Substances 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 12
- SQNZJJAZBFDUTD-UHFFFAOYSA-N durene Chemical compound CC1=CC(C)=C(C)C=C1C SQNZJJAZBFDUTD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010992 reflux Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 6
- 125000003118 aryl group Chemical group 0.000 claims description 4
- 238000007710 freezing Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 125000001624 naphthyl group Chemical group 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 9
- 239000000243 solution Substances 0.000 description 8
- 239000000575 pesticide Substances 0.000 description 5
- 239000003849 aromatic solvent Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000003995 emulsifying agent Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000000895 extractive distillation Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 2
- 241000238631 Hexapoda Species 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 coatings Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (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 high-purity production method of a high-solubility aromatic hydrocarbon solvent GF-S1800, which is used for removing C after durene10The heavy aromatics is used as raw material, and comprises the following steps: (1) washing with water; (2) rectifying by a first side line rectifying tower; (3) rectifying by a second side line rectifying tower; (4) and (4) treating the components. The high-purity production method of the high-solubility aromatic hydrocarbon solvent GF-S1800 has the advantages of ingenious design and novel conception, effectively removes impurities such as toluene, xylene and trimethylbenzene in raw materials by a process of washing and rectifying, and removes naphthalene by secondary rectification to obtain the low-naphthalene aromatic hydrocarbon solvent with high purity.
Description
Technical Field
The invention relates to the field of organic solvents, in particular to a high-purity production method of a high-solubility aromatic hydrocarbon solvent GF-S1800.
Background
The GF-S aromatic hydrocarbon solvent is C9、C10The heavy aromatic hydrocarbon is used as a raw material, is developed and produced by referring to international special aromatic hydrocarbon solvent standards, has the advantages of strong dissolving capacity, low toxicity, small smell, no oxygen and heavy metals, high boiling point, slow volatility and the like, and is mainly used in the industries of coatings, pesticides, plastics, coatings, paints and the like.
Because the GF-S aromatic hydrocarbon solvent has good gradient solubility for most pesticides, and has excellent intersolubility with pesticide emulsifier monomers, and the prepared missible oil has the characteristics of high flash point, slow volatilization speed, strong permeability and the like, the GF-S aromatic hydrocarbon solvent is often used as a pesticide emulsifier to prolong the retention time of pesticide drops on the surface of plants or insects so as to improve the pesticide effect.
The aromatic hydrocarbon solvent GF-S1800 has higher solubility and has wide prospect in the fields of high-grade baking varnish solvents, insecticides, emulsifiers, plasticizers and rubber resin solvents. However, the aromatic solvent GF-S1800 prepared by the prior production process still contains a certain amount of impurities, such as naphthalene, toluene, xylene and trimethylbenzene, which affect the use performance of the aromatic solvent.
Disclosure of Invention
The invention mainly solves the technical problem of providing a high-purity production method of a high-solubility aromatic hydrocarbon solvent GF-S1800, which can solve the problems of the existing production method.
In order to solve the technical problems, the invention adopts a technical scheme that: provides a high-purity production method of high-solubility aromatic hydrocarbon solvent GF-S1800 for removing C after durene10The heavy aromatics is used as raw material, and comprises the following steps:
(1) and (3) water washing treatment: introducing the raw materials into a washing tower for washing treatment so as to enable the raw materials to be in full contact with water;
(2) rectifying by a first side line rectifying tower: introducing the washed raw materials into a first side line rectifying tower for rectification, controlling the rectification process of the first side line rectifying tower, collecting a first component from the tower top, and collecting a second component from the side line;
(3) and (3) rectifying by using a second side line rectifying tower: introducing the tower bottom distillate of the first rectifying tower into a second side-line rectifying tower, controlling the rectifying process of the second side-line rectifying tower, collecting a third component from the tower top, and collecting the high-solubility aromatic hydrocarbon solvent GF-S1800 from a side line;
(4) component treatment: extracting, separating and recovering the first component and the second component, and freezing and crystallizing to recover the third component.
In a preferred embodiment of the present invention, in the step (1), the washing conditions of the washing tower are as follows: the pressure is 5-10 KPa, and the mass ratio of water to the raw materials is 1: 2 to 5.
In a preferred embodiment of the present invention, in the step (2), the rectification conditions of the first side line rectification column are as follows: the temperature of the top of the tower is 80-105 ℃, the temperature of the bottom of the tower is 150-170 ℃, the pressure is 80-110 KPa, and the reflux ratio is 1: 3-1: 6.
In a preferred embodiment of the present invention, in the step (3), the rectification conditions of the second side line rectification column are as follows: the temperature of the top of the tower is 150-190 ℃, the temperature of the bottom of the tower is 240-300 ℃, the pressure is 15-20 KPa, and the reflux ratio is 1: 8-1: 10.
In a preferred embodiment of the invention, the first component is an azeotropic mixture of water vapor with toluene and xylene; the second component is concentrated trimethylbenzene solution; the third component is a naphthalene enrichment solution; the fourth component is a high-solubility aromatic hydrocarbon solvent GF-S1800.
In a preferred embodiment of the invention, the main quality indexes of the high-solubility aromatic hydrocarbon solvent GF-S1800 are that the appearance is colorless transparent liquid, the initial ignition point is 210 ℃, the 98 percent distillation temperature is 243 ℃, and the density at 20 ℃ is 0.948g/cm3Closed flash point: 88 ℃, aromatic content: not less than 98.6%, naphthalene content: less than or equal to 25.7 percent.
The invention has the beneficial effects that: the high-purity production method of the high-solubility aromatic hydrocarbon solvent GF-S1800 has the advantages of ingenious design and novel conception, effectively removes impurities such as toluene, xylene and trimethylbenzene in raw materials by a process of washing and rectifying, and removes naphthalene by secondary rectification to obtain the low-naphthalene aromatic hydrocarbon solvent with high purity.
Drawings
FIG. 1 is a schematic process flow diagram of the high purity production process of the highly soluble aromatic solvent GF-S1800 of the present invention;
the parts in the drawings are numbered as follows: 1. the method comprises the following steps of (1) a water washing tower, (2) a first side line rectifying tower, (3) a second side line rectifying tower, (4) a raw material, (5) a first component, (6) a second component, (7) a third component, (8) a high-solubility aromatic hydrocarbon solvent GF-S1800, (9) a first extraction rectifying tower, (10) a second extraction rectifying tower, (11) a crystallization kettle, (12) toluene, (13) xylene and (14) trimethylbenzene.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
Referring to fig. 1, an embodiment of the present invention includes:
example 1
C after durene removal10The heavy aromatic raw material is controlled to have good flow rate by a feed pump and a flow rate adjusting device, and is pumped into a spray water washing tower 1 by a pipeline in a continuous feeding mode, and the mass ratio of water to the raw material is 1: 2, the raw materials are fully contacted with water, so that a small amount of impurity components of toluene and xylene in the raw materials are dissolved in the water, and an azeotrope is formed with water vapor in the subsequent rectification and is separated together; then introducing the washed raw materials into a first side line rectifying tower with the diameter of 1.6 m, the height of the tower of 34m, the number of tower plates of 45 and the filler of a metal wire mesh through a pipeline, setting and controlling the temperature of the top of the tower to be 80 ℃, the temperature of the bottom of the tower to be 150 ℃, the pressure to be 80KPa and the reflux ratio to be 1:3, collecting azeotrope of water vapor, toluene and xylene at the top of the tower, collecting trimethyl benzene enrichment liquid at the side line, introducing the distillate at the bottom of the tower to a second side line rectifying tower with the diameter of 1.8 m, the height of the tower to be 36m, the number of the tower plates to be 55 and the filler of the metal wire mesh, collecting the naphthalene enrichment liquid at the top of the second side line rectifying tower in a vacuumizing state of 15KPa, heating a material reboiler (supplying heat by a heat-conducting oil furnace), adjusting and controlling the temperature of the top of the tower to be 150 ℃, the temperature of the bottom of the tower to be.
The two-step rectification process has the following functions: the first side line rectifying tower is used for rectifying, so that impurities such as toluene, xylene and trimethylbenzene in the raw materials are effectively removed, and the defect that the existing aromatic hydrocarbon solvent contains impurities such as benzene, xylene and trimethylbenzene is overcome; and the second side line rectifying tower is used for rectifying to effectively remove the naphthalene in the aromatic solvent.
The main quality indexes of the obtained high-solubility aromatic hydrocarbon solvent GF-S1800 are as follows:
appearance: a colorless transparent liquid;
initial burdening point: at 210 ℃;
98% distillation temperature: 243 ℃;
density at 20 ℃:0.948g/cm3；
Closed flash point: 88 ℃;
aromatic hydrocarbon content: more than or equal to 98.6 percent;
naphthalene content: less than or equal to 25.7 percent.
In addition, the azeotrope of water vapor, toluene and xylene is extracted, separated and recovered, and the specific method comprises the following steps: after an azeotrope of water vapor, toluene and xylene is condensed, introducing the condensed azeotrope into a first extractive distillation tower, taking a mixed solution of glycerol and sulfolane as an extracting agent, and extracting the toluene with the purity of more than 98% from the top of the tower and the xylene with the purity of more than 98.8% from a lateral line under the conditions that the pressure is 80-100 KPa, the temperature at the top of the tower is 100-115 ℃, the temperature at the bottom of the tower is 200-210 ℃, the reflux ratio is 1:15 and the solvent ratio is 0.8.
The extraction separation and recovery of the concentrated trimethylbenzene solution are carried out by the specific method: condensing the concentrated trimethylbenzene solution, introducing the concentrated trimethylbenzene solution into a second extractive distillation tower, and collecting trimethylbenzene with the concentration of more than 95% from a side line under the conditions that the pressure is 90-100 KPa, the temperature at the top of the tower is 140-155 ℃, the temperature at the bottom of the tower is 200-210 ℃, the reflux ratio is 1:10 and the solvent ratio is 4 by taking N-methyl pyrrolidone and sulfolane as extracting agents.
The method comprises the following steps of (1) carrying out freezing crystallization on the naphthalene enrichment solution, and recovering naphthalene: introducing the naphthalene enrichment solution into a naphthalene crystallization kettle, cooling and crystallizing by using circulating cooling water, and then carrying out centrifugal separation.
Example 2
The difference from example 1 is that C after durene removal is added9The heavy aromatic raw material is controlled to have good flow rate by a feed pump and a flow rate adjusting device, and is pumped into a spray water washing tower 1 by a pipeline in a continuous feeding mode, and the mass ratio of water to the raw material is 1: 5, performing water washing treatment under the condition of fully contacting with water, so that a small amount of impurity components of toluene and xylene in the raw material are dissolved in the water, and are separated together with water vapor to form an azeotrope in the subsequent rectification; then introducing the washed raw materials into a first side line rectifying tower with the diameter of 1.6 m, the height of the tower of 34m, the number of tower plates of 45 and the filler of a metal wire mesh through a pipeline, setting and controlling the temperature at the top of the tower to be 105 ℃, the temperature at the bottom of the tower to be 170 ℃, the pressure to be 110KPa and the reflux ratio to be 1:6, collecting an azeotrope of water vapor, toluene and xylene at the top of the tower, collecting a trimethylbenzene concentrated solution at the side line, introducing the distillate at the bottom of the tower into a second side line rectifying tower with the diameter of 1.8 m, the height of the tower to be 36m, the number of tower plates ofIn the tower and the second side line rectifying tower, the material is heated by a reboiler (heated by a heat conducting oil furnace) under the vacuum state of 20kPa, the temperature at the top of the tower is adjusted and controlled at 190 ℃, the temperature at the bottom of the tower is 300 ℃, the reflux ratio is 1:10, naphthalene enriched liquid is collected at the top of the tower, a high-solubility aromatic hydrocarbon solvent GF-S1800 is collected at the side line, and the condensed and recovered liquid enters a product tank.
In the above embodiment, the impurities such as toluene, xylene, trimethylbenzene, naphthalene and the like in the raw material are effectively separated sequentially by water washing and twice distillation treatment to obtain the aromatic hydrocarbon solvent GF-S1800 with high purity, and the obtained impurity fraction is effectively recovered and utilized by the subsequent extractive distillation and freeze crystallization processes.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (5)
1. A high-purity production method of a high-solubility aromatic hydrocarbon solvent GF-S1800 takes C10 heavy aromatic hydrocarbon after durene removal as a raw material, and is characterized by comprising the following steps:
(1) and (3) water washing treatment: introducing the raw materials into a washing tower for washing treatment so as to enable the raw materials to be in full contact with water;
(2) rectifying by a first side line rectifying tower: introducing the washed raw materials into a first side line rectifying tower for rectification, controlling the rectification process of the first side line rectifying tower, collecting a first component from the tower top, and collecting a second component from the side line;
(3) and (3) rectifying by using a second side line rectifying tower: introducing the tower bottom distillate of the first side line rectifying tower into a second side line rectifying tower, controlling the rectifying process of the second side line rectifying tower, collecting a third component from the tower top, and collecting the high-solubility aromatic hydrocarbon solvent GFS1800 from a side line;
(4) component treatment: extracting, separating and recovering the first component and the second component, and freezing and crystallizing to recover the third component;
the high-solubility aromatic hydrocarbon solventThe main quality indexes of the GF-S1800 are that the appearance is colorless transparent liquid, the initial boiling point is 210 ℃, the 98 percent distillation temperature is 243 ℃, and the density at 20 ℃ is 0.948g/cm3Closed flash point: 88 ℃, aromatic content: not less than 98.6%, naphthalene content: less than or equal to 25.7 percent.
2. The process for the production of high purity of GF-S1800 as claimed in claim 1, wherein in the step (1), the washing conditions of the water washing column are: the pressure is 5-10 KPa, and the mass ratio of water to the raw materials is 1: 2 to 5.
3. The high purity production process of high solubility aromatic hydrocarbon solvent GF-S1800 as set forth in claim 1, wherein in said step (2), the distillation conditions of said first side-stream distillation column are: the temperature of the top of the tower is 80-105 ℃, the temperature of the bottom of the tower is 150-170 ℃, the pressure is 80-110 KPa, and the reflux ratio is 1: 3-1: 6.
4. The high purity production process of high solubility aromatic hydrocarbon solvent GF-S1800 as set forth in claim 1, wherein in said step (3), the rectification conditions of said second side-stream rectification column are: the temperature of the top of the tower is 150-190 ℃, the temperature of the bottom of the tower is 240-300 ℃, the pressure is 15-20 KPa, and the reflux ratio is 1: 8-1: 10.
5. The process for the production of high purity of the highly soluble aromatic hydrocarbon solvent GF-S1800 as claimed in claim 1 wherein the first component is an azeotropic mixture of water vapor with toluene and xylene; the second component is concentrated trimethylbenzene solution; the third component is a naphthalene enrichment solution; the fourth component is a high-solubility aromatic hydrocarbon solvent GF-S1800.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1017632A (en) * | 1961-11-10 | 1966-01-19 | Snam Spa | Process for the extraction in liquid phase of aromatic hydrocarbons from hydrocarbon mixtures containing them |
| CN101318874A (en) * | 2008-06-18 | 2008-12-10 | 常熟市联邦化工有限公司 | Process for joint production of aromatic solvent, stone oil naphthalin and durene line products with C10 heavy aromatic raw material |
| CN101538185A (en) * | 2009-04-14 | 2009-09-23 | 中国石化扬子石油化工有限公司 | Method for extracting mesitylene fraction rich in hydrocracking C 9 by combination of continuous lateral line distillation and extractive distillation |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1017632A (en) * | 1961-11-10 | 1966-01-19 | Snam Spa | Process for the extraction in liquid phase of aromatic hydrocarbons from hydrocarbon mixtures containing them |
| CN101318874A (en) * | 2008-06-18 | 2008-12-10 | 常熟市联邦化工有限公司 | Process for joint production of aromatic solvent, stone oil naphthalin and durene line products with C10 heavy aromatic raw material |
| CN101538185A (en) * | 2009-04-14 | 2009-09-23 | 中国石化扬子石油化工有限公司 | Method for extracting mesitylene fraction rich in hydrocracking C 9 by combination of continuous lateral line distillation and extractive distillation |
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Effective date of registration: 20210817 Address after: 215500 No. 33, Mogan Road, Mocheng street, Changshu City, Suzhou City, Jiangsu Province Patentee after: CHANGSHU CHANGJIANG STAINLESS STEEL MATERIAL Co.,Ltd. Address before: 215500 5th floor, building 4, 68 Lianfeng Road, Changfu street, Changshu City, Suzhou City, Jiangsu Province Patentee before: Changshu intellectual property operation center Co.,Ltd. |