CN113717032A - Process and device for controlling methanol rectification acid removal and pH value - Google Patents
Process and device for controlling methanol rectification acid removal and pH value Download PDFInfo
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- CN113717032A CN113717032A CN202111094935.7A CN202111094935A CN113717032A CN 113717032 A CN113717032 A CN 113717032A CN 202111094935 A CN202111094935 A CN 202111094935A CN 113717032 A CN113717032 A CN 113717032A
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- tail gas
- methanol
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 195
- 239000002253 acid Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000010992 reflux Methods 0.000 claims abstract description 69
- 238000005406 washing Methods 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 239000007791 liquid phase Substances 0.000 claims abstract description 14
- 239000012808 vapor phase Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 150000002148 esters Chemical class 0.000 claims description 18
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 238000005192 partition Methods 0.000 claims 1
- 230000002265 prevention Effects 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 9
- 239000000047 product Substances 0.000 description 22
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000009833 condensation Methods 0.000 description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000012263 liquid product Substances 0.000 description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
Images
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process and a device for controlling methanol rectification acid removal and pH value. The pre-tower reflux groove is provided with a left groove and a right groove, the top of the methanol rectification pre-tower discharges to a first condenser, a vapor phase product of the first condenser is connected with a second condenser, and a liquid phase product of the first condenser is connected with the left groove of the pre-tower reflux groove; the vapor phase product of the second condenser enters a tail gas washing tower, and the liquid phase product of the second condenser is connected with the left groove of the pre-tower reflux groove; taking water as an extracting agent, absorbing light components in a raw material liquid, taking the light components as non-condensed steam, and extracting the light components through a non-condensed steam pipe, wherein a liquid-phase product of a tail gas washing tower is connected with a right tank of a pre-tower reflux tank, a small amount of alkali liquor is introduced into a middle section of the tail gas washing tower and is connected, and a side-line extracted product is connected with a left tank of the pre-tower reflux tank; and the product in the left tank of the pre-tower reflux tank flows back to the methanol rectification pre-tower, and the product mainly containing methanol oil in the right tank of the pre-tower reflux tank flows out of the system. The invention accurately controls the PH value of the system and can effectively improve the treatment effect of methanol rectification acid removal.
Description
Technical Field
The invention belongs to the technical field of methanol rectification, and particularly relates to a process and a device for controlling acid removal and pH value of methanol rectification.
Background
Methanol is a chemical basic raw material with wide application, is applied to various fields such as fine chemical engineering, high molecules, pesticides, medicines, energy and the like, and has an important position in the international chemical industry market.
The pre-rectification process of the existing crude methanol is mainly finished in a pre-tower, and the pre-rectification aims to remove low-boiling components such as dimethyl ether and methyl formate contained in the crude methanol and non-condensed light components dissolved in the crude methanol, which have great influence on the quality of the subsequent rectification product of the methanol.
At present, extraction water of a rectification system is fed with crude methanol and is added into a pre-tower from the middle upper section of the pre-tower, impurity azeotrope accumulated in the top of the pre-tower and reflux cannot be effectively separated in the adding mode, and the reflux reaches a tower kettle, so that more crude alcohol impurities enter a subsequent refining process, and the product quality is seriously influenced.
The esterification reaction is more dominant than the hydrolysis reaction in the pre-tower, when the extraction water is added, the acid is generated by the change of the equilibrium, the acid is enriched at the top of the pre-tower and at the bottom of the tail gas washing tower, and the influence of the acidity on the product quality is very critical.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides a process and a device for controlling methanol rectification acid removal and pH value.
The technical scheme of the invention is a process for controlling methanol rectification acid removal and pH value, which comprises the following steps:
1) the vapor phase at the top of the methanol rectifying pre-tower T1 flows to a first condenser C1, the vapor phase condensed by the first condenser C1 flows to a second condenser C2, and the liquid phase of the first condenser C1 flows into a left groove V1L of a pre-tower reflux groove;
2) the vapor phase of the second condenser C2 is taken as raw material liquid to enter a tail gas washing tower T2, and the liquid phase of the second condenser C2 flows into a left groove V1L of the pre-tower reflux groove;
3) taking water as an extracting agent, absorbing light components in a raw material liquid, and then extracting the light components as non-condensed steam, wherein a bottom material of a tail gas washing tower T2 flows into a right groove V1R of a pre-tower reflux groove, a small amount of alkali liquor is introduced into the middle section of the tail gas washing tower, and the side-stream extracted water is output to a left groove V1L of the pre-tower reflux groove; the reflux liquid collected by the left groove V1L of the pre-tower reflux groove is refluxed to the top of a T1 pre-tower of the methanol rectification, and the product mainly comprising methanol oil in the right groove V1R) of the pre-tower reflux groove flows out of the system.
Further, the tail gas scrubbing tower T2 adopts a two-stage structure:
the methanol in the tail gas is washed by the extraction water at the upper section of the tail gas washing tower T2, so that the yield of the methanol is increased;
the lower section of the tail gas washing tower T2 strengthens the hydrolysis reaction of the esters, so that the esters form a high-concentration acid solution.
Further, a small amount of alkaline aqueous solution is adopted in the tail gas washing tower T2 to firstly react with the ester which is not condensed, the acid enrichment process and the ester neutralization reaction are synchronously carried out, and the enriched acid is discharged out of the system along with the methanol oil through the right groove V1R of the pre-tower reflux groove.
The second technical scheme of the invention is a device for removing the methanol rectification acid and controlling the pH value based on the process, which comprises a methanol rectification pre-tower T1, a first condenser C1, a second condenser C2, a pre-tower reflux tank V1, a tail gas washing tower T2 and a DCS control system.
The pre-tower reflux groove V1 is provided with a left groove and a right groove, and is a pre-tower reflux groove left groove V1L and a pre-tower reflux groove right groove V1R.
The top discharge of the methanol rectification pre-tower T1 is connected with a first condenser C1 through a pipeline S1, a vapor phase product of the first condenser C1 is connected with a second condenser C2, and a liquid phase product of the first condenser C1 is connected with a left groove V1L of a pre-tower reflux groove; a vapor-phase product of the second condenser C2 is used as a raw material liquid to enter a tail gas washing tower T2, and a liquid-phase product of the second condenser C2 is connected with a left groove V1L of a pre-tower reflux groove; taking water as an extracting agent, absorbing light components in a raw material liquid, taking the light components as non-condensed steam, and then extracting the light components through a non-condensed steam pipe S5, wherein a tail gas washing tower T2 liquid product is connected with a right tank V1R of a pre-tower reflux tank through a pipeline S2, a small amount of alkali liquor is connected with the middle section of the tail gas washing tower through an alkali liquor pipe, and a side-line extracted product is connected with a left tank V1L of the pre-tower reflux tank through a pipeline VI; the product in the left tank V1L of the pre-tower reflux tank is used as reflux liquid and is connected with a methanol rectification pre-tower T1 through a pipeline S3, and the product which mainly comprises methanol oil in the right tank V1R of the pre-tower reflux tank flows out of the system through a pipeline S4.
The pipeline S1 is provided with a flow meter FL, the pipeline S3 and the pipeline S4 are provided with a liquid level meter LG1 and a liquid level meter LG2, and the flow meter FL, the liquid level meter LG1 and the liquid level meter LG2 are connected with a DCS control system.
The scheme has the following characteristics:
1. the tail gas washing tower adopts a two-section structure, and the upper section of the tail gas washing tower adopts extraction water to wash methanol in the tail gas, so that the methanol yield is increased; the lower segment strengthens the hydrolysis reaction of the esters, so that the esters form a high-concentration acid solution;
2. the pre-tower reflux groove V1 is provided with a left groove and a right groove which are separated by a clapboard;
3. introducing a small amount of alkaline aqueous solution into the lower section of the tail gas washing tower to strengthen the hydrolysis reaction of esters, wherein the acid enrichment process and the ester neutralization reaction are synchronously carried out, and the enriched acid is discharged out along with the methanol oil through a pipeline S2 and a right groove V1R of a pre-tower reflux groove;
4. the non-condensed pipe S5 is provided with a structure for preventing the backflow of condensed liquid; the reflux system of the pre-rectifying tower is upgraded by adopting SUS304 material.
Advantageous effects
1. The tail gas washing tower adopts a two-stage absorption method, and the methanol yield can be increased through physical absorption; and then the hydrolysis reaction of the esters is strengthened through a chemical reaction, so that the effect of acid enrichment can be better achieved.
2. The baffle is arranged in the pre-tower reflux groove, so that the acid enriched at the bottom of the tail gas absorption tower and the crude methanol to be refluxed can be effectively separated, and the treatment effect of removing the methanol rectification acid is improved.
3. The PH value of a methanol rectification pre-tower system can be effectively controlled to be 7-9 by controlling the addition of the alkaline water solution and monitoring the liquid level of the pre-tower reflux tank by the liquid level meter, and the quality of a methanol product is improved.
4. The addition of the anti-condensation liquid backflow structure enables the non-condensation treatment to be more effective, and the treatment effect of removing the methanol rectification acid is also greatly influenced.
5. After the method is put into use, the technical problem that the quality of the methanol product is seriously influenced because the acid enters the pressurizing tower from the bottom of the tower and is esterified at high temperature in the prior art is thoroughly solved, and the qualification rate of the methanol product is greatly improved.
Drawings
FIG. 1 is a schematic diagram of a methanol rectification acid removal and pH control device;
wherein: the device comprises a methanol rectification pre-tower-T1, a first condenser-C1, a second condenser-C2, a pre-tower reflux tank-V1, a tail gas washing tower-T2, a pre-tower reflux tank left tank-V1L, a pre-tower reflux tank right tank-V1R, a pipeline I-S1, a pipeline II-S2, a pipeline III-S3, a pipeline IV-S4, an uncondensed pipe-S5, a pipeline VI-S6, a flow meter-FL, a liquid level meter I-LG 1 and a liquid level meter II-LG 2.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
example 1
As shown in FIG. 1, the pre-column reflux drum V1 has two slots, i.e., a left pre-column reflux drum V1L and a right pre-column reflux drum V1R.
The process flow comprises the following steps: the top discharge of the methanol rectification pre-tower T1 is connected with a first condenser C1 through a pipeline S1, a vapor phase product of the first condenser C1 is connected with a second condenser C2, and a liquid phase product of the first condenser C1 is connected with a left groove V1L of a pre-tower reflux groove; a vapor-phase product of the second condenser C2 is used as a raw material liquid to enter a tail gas washing tower T2, and a liquid-phase product of the second condenser C2 is connected with a left groove V1L of a pre-tower reflux groove; taking water as an extracting agent, absorbing light components in a raw material liquid, taking the light components as non-condensed steam, and then extracting the light components through a non-condensed steam pipe S5, wherein a tail gas washing tower T2 liquid product is connected with a right tank V1R of a pre-tower reflux tank through a pipeline S2, a small amount of alkali liquor is connected with the middle section of the tail gas washing tower through an alkali liquor pipe, and a side-line extracted product is connected with a left tank V1L of the pre-tower reflux tank through a pipeline VI; the product in the left tank V1L of the pre-tower reflux tank is used as reflux liquid and is connected with a methanol rectification pre-tower T1 through a pipeline S3, and the product which mainly comprises methanol oil in the right tank V1R of the pre-tower reflux tank flows out of the system through a pipeline S4.
The pipeline S1 is provided with a flow meter FL, the pipeline S3 and the pipeline S4 are provided with a liquid level meter LG1 and a liquid level meter LG2, and the flow meter FL, the liquid level meter LG1 and the liquid level meter LG2 are connected with a DCS control system.
The tail gas washing tower T2 adopts a two-section structure, and the upper section of the tail gas washing tower T2 adopts extraction water to wash methanol in the tail gas, so that the methanol yield can be increased; the lower section of the tail gas washing tower T2 strengthens the hydrolysis reaction of the esters, so that the esters form a high-concentration acid solution, and the acid enrichment effect can be better achieved.
A small amount of alkaline aqueous solution is adopted in the tail gas washing tower to firstly react with esters which are not condensed, then the acid enrichment process and the ester neutralization reaction are synchronously carried out, and the enriched acid passes through a pipeline S2 and a pre-tower reflux groove right groove V1R and is discharged along with methanol oil.
The non-condensed pipe S5 is provided with a structure for preventing the backflow of condensed liquid; the addition of the anti-condensation liquid backflow structure enables the non-condensation treatment to be more effective, and the treatment effect of removing the methanol rectification acid is also greatly influenced. The reflux system of the pre-rectifying tower is upgraded by adopting SUS304 material. The tail gas washing tower adopts a two-stage absorption method, and the methanol yield can be increased through physical absorption; and then the hydrolysis reaction of the esters is strengthened through a chemical reaction, so that the effect of acid enrichment can be better achieved. The baffle is arranged in the pre-tower reflux groove, so that the acid enriched at the bottom of the tail gas absorption tower and the crude methanol to be refluxed can be effectively separated, and the treatment effect of removing the methanol rectification acid is improved. The PH value of a methanol rectification pre-tower system can be effectively controlled by controlling the addition of the alkaline water solution and monitoring the liquid level of the pre-tower reflux tank by the liquid level meter, and the quality of a methanol product is improved.
Claims (7)
1. A process for controlling methanol rectification acid removal and pH value is characterized by comprising the following steps:
1) the vapor phase at the top of the methanol rectifying pre-tower (T1) is sent to a first condenser (C1), the vapor phase condensed by the first condenser (C1) is sent to a second condenser (C2), and the liquid phase of the first condenser (C1) flows into a left tank (V1L) of a pre-tower reflux tank;
2) the vapor phase of the second condenser (C2) is used as a raw material liquid to enter a tail gas washing tower (T2), and the liquid phase of the second condenser (C2) flows into a left groove (V1L) of a pre-tower reflux groove;
3) taking water as an extracting agent, absorbing light components in a raw material liquid, and then extracting the light components as non-condensed steam, wherein a tower bottom material of a tail gas washing tower (T2) flows into a right groove (V1R) of a pre-tower reflux groove, a small amount of alkali liquor is introduced into a middle section of the tail gas washing tower, and a side-stream is extracted and output to a left groove (V1L) of the pre-tower reflux groove; the reflux liquid collected by the left groove (V1L) of the pre-tower reflux groove is refluxed to the top of the methanol rectification pre-tower (T1), and the product mainly comprising methanol oil in the right groove (V1R) of the pre-tower reflux groove flows out of the system.
2. The process for controlling the removal of methanol rectification acid and the pH value according to claim 1, wherein the tail gas washing tower (T2) adopts a two-stage structure:
the upper section of the tail gas washing tower (T2) adopts extraction water to wash the methanol in the tail gas, thereby increasing the yield of the methanol;
the lower section of the tail gas washing tower (T2) strengthens the hydrolysis reaction of the esters, so that the esters form a high-concentration acid solution.
3. The process for controlling the removal of acid and the pH value of methanol rectification according to claim 1, wherein a small amount of alkaline aqueous solution is adopted in the tail gas washing tower (T2) to react with the ester which is not condensed, the acid enrichment process and the ester neutralization reaction are carried out synchronously, and the enriched acid is discharged out of the system along with the methanol oil through the right groove (V1R) of the pre-tower reflux groove.
4. The plant of a process according to any one of claims 1 to 3, characterized by comprising a methanol rectification pre-column (T1), a first condenser (C1), a second condenser (C2), a pre-column reflux drum (V1), a tail gas wash column (T2) and a DCS control system;
the pre-tower reflux groove (V1) is provided with a left groove and a right groove which are respectively a left groove (V1L) and a right groove (V1R) of the pre-tower reflux groove;
the top discharge of the methanol rectification pre-tower (T1) is connected with a first condenser (C1) through a pipeline I (S1), a vapor phase outlet of the first condenser (C1) is connected with a second condenser (C2), and a liquid phase outlet of the first condenser (C1) is connected with a left groove (V1L) of a pre-tower reflux groove; a vapor phase outlet of the second condenser (C2) is used as a raw material liquid to enter a tail gas washing tower (T2), and a liquid phase outlet of the second condenser (C2) is connected with a left groove (V1L) of the pre-tower reflux groove;
non-condensed steam is extracted through a non-condensed pipe (S5), a liquid phase outlet of a tail gas washing tower (T2) is connected with a right tank (V1R) of a pre-tower reflux tank through a pipeline II (S2), a small amount of alkali liquor is connected with the middle section of the tail gas washing tower through an alkali liquor pipe, and a side-line extracted product is connected with a left tank (V1L) of the pre-tower reflux tank through a pipeline VI (S6); the reflux liquid in the left tank (V1L) of the pre-tower reflux groove is connected with a methanol rectification pre-tower (T1) through a pipeline III (S3), and the product flows out from the bottom of the right tank (V1R) of the pre-tower reflux groove;
be equipped with Flowmeter (FL) on pipeline I (S1), be equipped with level gauge I (LG1) and level gauge II (LG2) on pipeline III (S3) and pipeline IV (S4), Flowmeter (FL), level gauge I (LG1) and level gauge II (LG2) be connected with DCS control system.
5. The apparatus according to claim 4, wherein the noncondensable pipe (S5) is provided with a backflow prevention structure.
6. The device of claim 4, wherein the device is constructed of SUS304 upgrade.
7. The apparatus according to claim 4, wherein the two troughs, left and right, of the pre-tower reflux drum (V1) are separated by a partition.
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| CN202111094935.7A CN113717032B (en) | 2021-09-17 | 2021-09-17 | Process and device for controlling methanol rectifying acid removal and PH value |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111094935.7A CN113717032B (en) | 2021-09-17 | 2021-09-17 | Process and device for controlling methanol rectifying acid removal and PH value |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN204815742U (en) * | 2015-07-29 | 2015-12-02 | 兖矿国宏化工有限责任公司 | Methyl alcohol rectifier unit |
| CN106478370A (en) * | 2016-10-11 | 2017-03-08 | 东华工程科技股份有限公司 | A kind of method for reclaiming methyl alcohol in improved methanol rectification periodic off-gases |
| CN107522593A (en) * | 2017-08-10 | 2017-12-29 | 青海盐湖工业股份有限公司 | A kind of pre- distillation system of methanol |
| CN107778143A (en) * | 2017-09-19 | 2018-03-09 | 中建安装工程有限公司 | A kind of low-temp methanol washes the device and method of recycle methanol dividing plate extractive distillation column desulfurization |
| CN208166887U (en) * | 2018-03-30 | 2018-11-30 | 山西焦化股份有限公司 | A kind of methanol rectification pre-tower backflash extraction equipment |
| CN109134196A (en) * | 2018-07-31 | 2019-01-04 | 东华工程科技股份有限公司 | The system of methanol is recycled in a kind of improved methanol rectification periodic off-gases |
-
2021
- 2021-09-17 CN CN202111094935.7A patent/CN113717032B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204815742U (en) * | 2015-07-29 | 2015-12-02 | 兖矿国宏化工有限责任公司 | Methyl alcohol rectifier unit |
| CN106478370A (en) * | 2016-10-11 | 2017-03-08 | 东华工程科技股份有限公司 | A kind of method for reclaiming methyl alcohol in improved methanol rectification periodic off-gases |
| CN107522593A (en) * | 2017-08-10 | 2017-12-29 | 青海盐湖工业股份有限公司 | A kind of pre- distillation system of methanol |
| CN107778143A (en) * | 2017-09-19 | 2018-03-09 | 中建安装工程有限公司 | A kind of low-temp methanol washes the device and method of recycle methanol dividing plate extractive distillation column desulfurization |
| CN208166887U (en) * | 2018-03-30 | 2018-11-30 | 山西焦化股份有限公司 | A kind of methanol rectification pre-tower backflash extraction equipment |
| CN109134196A (en) * | 2018-07-31 | 2019-01-04 | 东华工程科技股份有限公司 | The system of methanol is recycled in a kind of improved methanol rectification periodic off-gases |
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