CN101712613B - Method for de-iodinating and refining acetic acid - Google Patents
Method for de-iodinating and refining acetic acid Download PDFInfo
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- CN101712613B CN101712613B CN 200810157532 CN200810157532A CN101712613B CN 101712613 B CN101712613 B CN 101712613B CN 200810157532 CN200810157532 CN 200810157532 CN 200810157532 A CN200810157532 A CN 200810157532A CN 101712613 B CN101712613 B CN 101712613B
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Abstract
The invention belongs to the field of refining chemical products, and particularly discloses a method for de-iodinating and refining acetic acid. The refining method comprises the following steps: absorbing an acetic acid finished product collected from a rectifying tower by an adsorbent or an ion exchange resin; reducing iodine in the acetic acid to below 10PPb; and reducing the content of formic acid to less than or equal to 30PPm. The refined acetic acid product obtained through the refining process meets the requirements of downstream high-end products and the requirements of high-end customers for producing vinyl acetate and the like.
Description
Technical field
The invention belongs to the Chemicals field of refinement, be specially a kind of method for de-iodinating and refining acetic acid.
Background technology
Acetic acid formal name used at school acetic acid, molecular formula C
2H
4O
2Acetic acid is a kind of important basic chemical raw materials, be widely used in the industry such as chemical industry, light industry, weaving, agricultural chemicals, medicine, electronics, food, for the production of vinyl acetate between to for plastic, polyvinyl alcohol, terephthalic acid, acetic ester, aceticanhydride etc., its derivative is nearly hundreds of.
The production method of acetic acid is, take carbon monoxide and methyl alcohol as raw material, produce with oxo synthesis, the method that adopts at present is the low-pressure methanol oxo synthesis, and this low pressure methanol oxo synthesis is take the iodate rhodium as catalyzer, the technological reaction mild condition, the about 3.4MPa of pressure, yield is higher, and the selectivity of methyl alcohol Dichlorodiphenyl Acetate reaches more than 99%, production cost is low, but the acetate products that this production method obtains contains iodine impurity.
At present, for above-mentioned production method, the Dichlorodiphenyl Acetate purification is processed the method steps that adopts and is, adds KOH and H in rectifying tower
3PO
2, obtain removing the acetate products of iodine.
Take off the acetate products that iodine obtains according to this kind treatment process, can remove the minimum PPm of the being down to level of iodide ion content, the content of formic acid is less than or equal to 0.03%, even follow the inspecting standard of GB/T1628.1-2000, the premium grads that obtains for this standard can not satisfy the quality requirement of high-end user, be merely able to satisfy the needs of common customer, for example: iodide ion content is below 10PPb in the need of production acetic acid of vinyl acetate between to for plastic, the acetate products that obtains with this treatment process can not be used in the production of vinyl acetate between to for plastic, so is badly in need of a kind of technology that can reduce iodine content in the acetic acid finished product.
Summary of the invention
Purpose of the present invention is exactly inadequate for above-mentioned Dichlorodiphenyl Acetate product purification processes precision, can not satisfy the needs of high-end user, particularly in order to reach the required acetate standard of vinyl acetate production, and provide a kind of Dichlorodiphenyl Acetate to carry out the method for de-iodinating and refining, this process for purification can not only be down to iodine content in the acetic acid vinyl acetate between to for plastic market demand for less than or equal to 10PPb, and can reduce formic acid content for less than or equal to 30PPm.
Method for de-iodinating and refining acetic acid of the present invention is: adsorb by sorbent material absorption and/or ion exchange resin from the finished product acetic acid of rectifying tower extraction, the iodine in the acetic acid is taken off to 10PPb.
Method for de-iodinating and refining acetic acid concrete steps of the present invention are: enter adsorption tower after the finished product acetic acid of rectifying tower extraction cools off, deviate from formic acid in the acetic acid through transshipping the absorption of silver-colored oxygenant, enter ion exchange tower by out acetic acid in the adsorption tower, absorption through polystyrene type ion exchange resin, remove the iodine in the acetic acid, obtain refining acetic acid, cooled off through interchanger by ion exchange tower acetic acid out, temperature is down to 30-50 ℃, then enters storage tank and stores.
Of the present invention year silver-colored oxygenant is silver nitrate solution, and its concentration is 0.05-0.2mol/L; Pressure in the adsorption tower is 0.2-0.5Mpa, and temperature is 40-138 ℃; Pressure in the ion exchange tower is 0.2-0.5Mpa, and temperature is 80-100 ℃; Acetic acid is 5:1-2 with the consumption weight ratio of carrying silver-colored oxygenant; The consumption weight ratio of acetic acid and ion exchange resin is 5:2-2.5.
It is operating as method for de-iodinating and refining acetic acid of the present invention in detail: after being cooled to 100 ℃ from the acetic acid of rectifying tower extraction, enter adsorption tower, pressure in the adsorption tower is 0.2-0.5Mpa, temperature is 40-138 ℃, deviate from formic acid in the acetic acid through transshipping the absorption of silver-colored oxygenant, enter ion exchange tower by out acetic acid in the adsorption tower, the pressure of this ion exchange tower is 0.2-0.5Mpa, temperature is 80-100 ℃, and the absorption through polystyrene type ion exchange resin removes the iodine in the acetic acid, obtain refining acetic acid, cooled off through interchanger by out acetic acid in the ion exchange tower, temperature is down to 30-50 ℃, then enters storage tank and stores.
The invention has the beneficial effects as follows that formic acid foreign matter content in the acetic acid can be down to below the 30PPm, iodine content is down to below the 10PPb.By the refining acetate products that this process for refining makes, meet the demand of downstream high-end product, can be used for the high-end clients' such as production of vinyl acetate between to for plastic demand.
The control case of foreign matter content is as shown in the table before and after refining:
| Dopant species | Before adopting present technique | After adopting present technique |
| Formic acid | ≤0.03％ | ≤30PPm |
| Iodine | The PPm level | ≤10PPb |
Description of drawings
Fig. 1 schema of the present invention.
Embodiment
Below in conjunction with drawings and Examples technical scheme of the present invention is further specified.
Embodiment 1
After being cooled to 100 ℃ from the acetic acid of rectifying tower extraction, enter adsorption tower, pressure in the adsorption tower is 0.2Mpa, temperature is 40 ℃, deviate from formic acid in the acetic acid through transshipping the absorption of silver-colored oxygenant, enter ion exchange tower by out acetic acid in the adsorption tower, the pressure of this ion exchange tower is 0.2Mpa, temperature is 80 ℃, and the absorption through polystyrene type ion exchange resin removes the iodine in the acetic acid, obtain refining acetic acid, cooled off through interchanger by ion exchange tower acetic acid out, temperature is down to 50 ℃, then enters storage tank and stores.
Embodiment 2
After being cooled to 100 ℃ from the acetic acid of rectifying tower extraction, enter adsorption tower, pressure in the adsorption tower is 0.5Mpa, temperature is 138 ℃, deviate from formic acid in the acetic acid through transshipping the absorption of silver-colored oxygenant, enter ion exchange tower by out acetic acid in the adsorption tower, the pressure of this ion exchange tower is 0.5Mpa, temperature is 100 ℃, and the absorption through polystyrene type ion exchange resin removes the iodine in the acetic acid, obtain refining acetic acid, cooled off through interchanger by ion exchange tower acetic acid out, temperature is down to 30 ℃, then enters storage tank and stores.
Claims (5)
1. method for de-iodinating and refining acetic acid, its concrete steps are: enter adsorption tower after the finished product acetic acid of rectifying tower extraction cools off, deviate from formic acid in the acetic acid through transshipping the absorption of silver-colored oxygenant, enter ion exchange tower by out acetic acid in the adsorption tower, absorption through polystyrene type ion exchange resin, remove the iodine in the acetic acid, obtain refining acetic acid, cooled off through interchanger by ion exchange tower acetic acid out, temperature is down to 30-50 ℃, then enter storage tank and store, the iodine in the acetic acid is taken off to 10PPb; Described year silver-colored oxygenant is silver nitrate solution.
2. method for de-iodinating and refining acetic acid according to claim 1, it is characterized in that: the concentration of described silver nitrate solution is 0.05-0.2mol/L.
3. method for de-iodinating and refining acetic acid according to claim 1 is characterized in that: the pressure in the described adsorption tower is 0.2-0.5Mpa, and temperature is 40-138 ℃.
4. method for de-iodinating and refining acetic acid according to claim 1 is characterized in that: the pressure in the described ion exchange tower is 0.2-0.5Mpa, and temperature is 80-100 ℃.
5. method for de-iodinating and refining acetic acid according to claim 1 is characterized in that: acetic acid is 5 with the consumption weight ratio of carrying silver-colored oxygenant: 1-2; The consumption weight ratio of acetic acid and ion exchange resin is 5: 2-2.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810157532 CN101712613B (en) | 2008-10-06 | 2008-10-06 | Method for de-iodinating and refining acetic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810157532 CN101712613B (en) | 2008-10-06 | 2008-10-06 | Method for de-iodinating and refining acetic acid |
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|---|---|
| CN101712613A CN101712613A (en) | 2010-05-26 |
| CN101712613B true CN101712613B (en) | 2013-03-27 |
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| CN 200810157532 Active CN101712613B (en) | 2008-10-06 | 2008-10-06 | Method for de-iodinating and refining acetic acid |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102371147B (en) * | 2010-08-23 | 2013-05-08 | 中国石油化工股份有限公司 | Preparation method of iodine removing agent |
| CN107986953B (en) * | 2017-12-06 | 2021-07-23 | 江苏索普化工股份有限公司 | Production device and production process for synthesizing acetic acid by methanol low-pressure carbonyl |
| CN116606204B (en) * | 2023-07-17 | 2023-10-20 | 成都普什医药塑料包装有限公司 | Recovered acetic acid for low-chroma acetic anhydride and cellulose acetate, and recovery method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4615806A (en) * | 1985-03-07 | 1986-10-07 | Celanese Corporation | Removal of iodide compounds from non-aqueous organic media |
| CN1743065A (en) * | 2005-07-27 | 2006-03-08 | 复旦大学 | Method for preparing in-situ silver-carried natural zeolite deiodinating adsorbent |
-
2008
- 2008-10-06 CN CN 200810157532 patent/CN101712613B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4615806A (en) * | 1985-03-07 | 1986-10-07 | Celanese Corporation | Removal of iodide compounds from non-aqueous organic media |
| US4615806B1 (en) * | 1985-03-07 | 1994-05-03 | Hoechst Co American | Removal of iodide compounds from non-aqueous organic media |
| CN1743065A (en) * | 2005-07-27 | 2006-03-08 | 复旦大学 | Method for preparing in-situ silver-carried natural zeolite deiodinating adsorbent |
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| CN101712613A (en) | 2010-05-26 |
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Effective date of registration: 20170504 Address after: Zaozhuang City, Shandong province 277527 Mu Shi Zhen (Tengzhou Lunan high tech chemical park) Co-patentee after: Yankuang Group Ltd. Patentee after: Yankuang Lunan Chemical Co., Ltd. Address before: 277527 Shandong Province, Tengzhou City Stone Town Co-patentee before: Yankuang Group Ltd. Patentee before: Yancon Cathay Coal Chemicals Co., Ltd. |
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