CN109264684A - Nitric acid reclaiming clean technique - Google Patents
Nitric acid reclaiming clean technique Download PDFInfo
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- CN109264684A CN109264684A CN201811322333.0A CN201811322333A CN109264684A CN 109264684 A CN109264684 A CN 109264684A CN 201811322333 A CN201811322333 A CN 201811322333A CN 109264684 A CN109264684 A CN 109264684A
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- CN
- China
- Prior art keywords
- nitric acid
- liquid phase
- purifying column
- enters
- reclaiming clean
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- 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.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/38—Nitric acid
- C01B21/40—Preparation by absorption of oxides of nitrogen
Abstract
The invention discloses a kind of nitric acid reclaiming clean techniques, include the following steps: step 1: the liquid phase of the nitric acid of the methanol containing 21-85wt% and 0.5-12wt% that esterification is obtained is sent into nitric acid purifying column；Step 2: the nitric oxide that volume fraction is 5-100% being sent into nitric acid purifying column and is reacted；Step 3: liquid phase enters circulating pump after flowing out nitric acid purifying column, and after shunting, Partial Liquid Phase returns to purifying column, remaining liquid phase enters subsequent workshop section, and gas phase enters system circulation gas；The nitric acid purifying column is void tower, and it is 1:15-150 that the circulating pump, which enters the liquid phase of subsequent workshop section and enters the split ratio of the liquid phase of purifying column,.The invention has the benefit that the nitric acid reclaiming clean technique, which can be realized, is reduced to 0.1% or less for nitric acid content under 85-100 DEG C of lower temperature under the premise of catalyst is not used.
Description
Technical field
The present invention relates to ethylene glycol production technology, in particular to a kind of nitric acid reclaiming clean technique.
Background technique
Currently, the process route of heavy industrialization synthesis gas production ethylene glycol mainly uses two-step method, i.e., first with
Methyl nitrite and reaction of carbon monoxide generate dimethyl oxalate, and then Hydrogenation of Dimethyl Oxalate obtains ethylene glycol product.Wherein,
Methyl nitrite is reacted to obtain by nitric oxide, oxygen and methanol esterification.In the preparation process of methyl nitrite, side reaction is deposited
Causing to have nitric acid generation.In order to cut down the consumption of raw materials, sewage treatment burden is reduced, people carry out reclaiming clean to nitric acid.
Existing nitric acid reclaiming clean generallys use catalysis and goes back orthonitric acid purification process, realizes the relatively low temperature at 85-100 DEG C
Degree is lower to be reduced to 0.1% hereinafter, realizing nitric acid purification target substantially for nitric acid content using catalyst.But catalysis reduction nitre
Acid purification process requirement uses catalyst, and universal of catalyst life is one year, and the service life is shorter.Meanwhile the replacement of catalyst
Expense market price reaches more than 1,000 ten thousand yuan, with high costs, has much room for improvement.
Summary of the invention
The object of the present invention is to provide a kind of nitric acid reclaiming clean techniques.Under the premise of catalyst is not used, the nitric acid
Reclaiming clean technique, which can be realized, is reduced to 0.1% or less for nitric acid content under 85-100 DEG C of lower temperature.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of nitric acid reclaiming clean technique, includes the following steps:
Step 1: the liquid phase of the nitric acid of the methanol containing 21-85wt% and 0.5-12wt% that esterification is obtained is sent into nitric acid
Purifying column；
Step 2: the nitric oxide that volume fraction is 5-100% being sent into nitric acid purifying column and is reacted；
Step 3: liquid phase enters circulating pump after flowing out nitric acid purifying column, and after shunting, Partial Liquid Phase returns to purifying column, remaining fluid
Mutually enter subsequent workshop section, gas phase enters system circulation gas；
The nitric acid purifying column is void tower, and the circulating pump enters the liquid phase of subsequent workshop section and enters the shunting of the liquid phase of purifying column
Than being 1: 15-150.
The present invention is further arranged to: the ratio of height to diameter of the nitric acid purifying column is 1: 20-200.
The present invention is further arranged to: the nitric oxide is from system circulation gas or external introducing.
In conclusion the invention has the following advantages:
Under the premise of catalyst is not used, which can be realized will under 85-100 DEG C of lower temperature
Concentration of nitric acid decreases below 100ppm, while generating in methyl nitrite return system.
Detailed description of the invention
Fig. 1 is flow chart of the invention.
Appended drawing reference: 1, nitric acid purifying column；2, fluid inlet；3, gaseous phase outlet；4, circulation fluid entrance；5, gas phase import；
6, liquid-phase outlet；7, circulating pump.
Specific embodiment
Below in conjunction with attached drawing, invention is further described in detail.
Embodiment 1-5 is for illustrating nitric acid reclaiming clean technique.Embodiment 1-5 nitric acid reclaiming clean technique is specific as follows.
Referring to Fig.1, a kind of nitric acid reclaiming clean technique, includes the following steps:
Step 1: the liquid phase of the nitric acid of the methanol containing 21-85wt% and 0.5-12wt% that esterification is obtained from liquid phase into
Mouth 2 is sent into nitric acid purifying columns 1；
Step 2: net by nitric acid is sent into from gas phase import 5 from the nitric oxide that the volume fraction of system circulation gas is 5-100%
Change tower 1 to be reacted；
Step 3: liquid phase enters circulating pump 7 after flowing out nitric acid purifying column 1 from liquid-phase outlet 6, and after shunting, Partial Liquid Phase is from following
Ring liquid entrance 4 returns to purifying column, remaining liquid phase enters subsequent workshop section, and gas phase enters system circulation gas from gaseous phase outlet 3.
Nitric acid purifying column 1 is void tower, and circulating pump 7 enters the liquid phase of subsequent workshop section and enters the split ratio of the liquid phase of purifying column
It is 1: 15-150.The ratio of height to diameter of nitric acid purifying column 1 is 1: 20-200.
Table 1, embodiment 1-5 nitric acid reclaiming clean process parameter table
It detects embodiment 1-5 and enters nitric acid content in the liquid phase of subsequent workshop section.
Table 2, embodiment 1-5 enter concentration of nitric acid in the liquid phase of subsequent workshop section
As known from Table 2, nitric acid contains in the liquid phase into subsequent workshop section obtained using the nitric acid cleaning and recovering process of embodiment 1-5
Amount is respectively less than 100ppm.
The present embodiment is only explanation of the invention, is not limitation of the present invention, and those skilled in the art exist
It can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as in the present invention
Scope of the claims in all by the protection of Patent Law.
Claims (3)
1. a kind of nitric acid reclaiming clean technique, it is characterized in that: including the following steps:
Step 1: it is net that the liquid phase of the nitric acid of the methanol containing 21-85wt% and 0.5-12wt% that esterification is obtained is sent into nitric acid
Change tower (1)；
Step 2: the nitric oxide that volume fraction is 5-100% being sent into nitric acid purifying column (1) and is reacted；
Step 3: liquid phase flows out nitric acid purifying column (1) and enters circulating pump (7) afterwards, and after shunting, Partial Liquid Phase returns to purifying column,
Remaining liquid phase enters subsequent workshop section, and gas phase enters system circulation gas；
The nitric acid purifying column (1) is void tower, and the circulating pump (7) enters the liquid phase of subsequent workshop section and enters the liquid phase of purifying column
Split ratio be 1:15-150.
2. reclaiming clean technique according to claim 1, it is characterized in that: the ratio of height to diameter of the nitric acid purifying column (1) is 1:
20-200。
3. reclaiming clean technique according to claim 1, it is characterized in that: the nitric oxide from system circulation gas or
Outside introduces.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811322333.0A CN109264684A (en) | 2018-11-07 | 2018-11-07 | Nitric acid reclaiming clean technique |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811322333.0A CN109264684A (en) | 2018-11-07 | 2018-11-07 | Nitric acid reclaiming clean technique |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109264684A true CN109264684A (en) | 2019-01-25 |
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| CN201811322333.0A Pending CN109264684A (en) | 2018-11-07 | 2018-11-07 | Nitric acid reclaiming clean technique |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3281274A (en) * | 1962-09-14 | 1966-10-25 | Exxon Research Engineering Co | Electrochemical cell and method of regenerating nitric acid in an electrochemical cell |
| CN101190884A (en) * | 2006-11-21 | 2008-06-04 | 上海焦化有限公司 | Method for synthesizing dimethyl oxalate and coproducing dimethyl carbonate |
| CN106565494A (en) * | 2015-10-12 | 2017-04-19 | 中国石油化工股份有限公司 | Methyl nitrite preparation method by reaction of NO and nitric acid and methanol |
| CN106748785A (en) * | 2016-12-14 | 2017-05-31 | 上海华谊能源化工有限公司 | Waste water treatment process and system in a kind of synthesis gas preparing ethylene glycol technique |
| CN106904714A (en) * | 2017-02-14 | 2017-06-30 | 新疆天智辰业化工有限公司 | Nitrate reductase purification technique in coal-ethylene glycol production |
| CN106955649A (en) * | 2017-03-23 | 2017-07-18 | 宁波中科远东催化工程技术有限公司 | A kind of nitrate reductase device |
| CN107033004A (en) * | 2017-05-31 | 2017-08-11 | 西安汉术化学工程股份有限公司 | Nitrate reductase method in methyl nitrite preparation process |
| CN206731083U (en) * | 2017-04-28 | 2017-12-12 | 宁波中科远东催化工程技术有限公司 | A kind of synthesis gas preparing ethylene glycol technique nitrate reductase purifying column |
| CN108620107A (en) * | 2018-06-23 | 2018-10-09 | 宁波中科远东催化工程技术有限公司 | A kind of catalyst and its preparation method and application for Hydrogenation of Dimethyl Oxalate synthesizing methyl glycolate |
-
2018
- 2018-11-07 CN CN201811322333.0A patent/CN109264684A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3281274A (en) * | 1962-09-14 | 1966-10-25 | Exxon Research Engineering Co | Electrochemical cell and method of regenerating nitric acid in an electrochemical cell |
| CN101190884A (en) * | 2006-11-21 | 2008-06-04 | 上海焦化有限公司 | Method for synthesizing dimethyl oxalate and coproducing dimethyl carbonate |
| CN106565494A (en) * | 2015-10-12 | 2017-04-19 | 中国石油化工股份有限公司 | Methyl nitrite preparation method by reaction of NO and nitric acid and methanol |
| CN106748785A (en) * | 2016-12-14 | 2017-05-31 | 上海华谊能源化工有限公司 | Waste water treatment process and system in a kind of synthesis gas preparing ethylene glycol technique |
| CN106904714A (en) * | 2017-02-14 | 2017-06-30 | 新疆天智辰业化工有限公司 | Nitrate reductase purification technique in coal-ethylene glycol production |
| CN106955649A (en) * | 2017-03-23 | 2017-07-18 | 宁波中科远东催化工程技术有限公司 | A kind of nitrate reductase device |
| CN206731083U (en) * | 2017-04-28 | 2017-12-12 | 宁波中科远东催化工程技术有限公司 | A kind of synthesis gas preparing ethylene glycol technique nitrate reductase purifying column |
| CN107033004A (en) * | 2017-05-31 | 2017-08-11 | 西安汉术化学工程股份有限公司 | Nitrate reductase method in methyl nitrite preparation process |
| CN108620107A (en) * | 2018-06-23 | 2018-10-09 | 宁波中科远东催化工程技术有限公司 | A kind of catalyst and its preparation method and application for Hydrogenation of Dimethyl Oxalate synthesizing methyl glycolate |
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Application publication date: 20190125 |