CN102824919A - Method for reducing oxidation catalyst in PTA production apparatus - Google Patents
Method for reducing oxidation catalyst in PTA production apparatus Download PDFInfo
- Publication number
- CN102824919A CN102824919A CN2011101586365A CN201110158636A CN102824919A CN 102824919 A CN102824919 A CN 102824919A CN 2011101586365 A CN2011101586365 A CN 2011101586365A CN 201110158636 A CN201110158636 A CN 201110158636A CN 102824919 A CN102824919 A CN 102824919A
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- CN
- China
- Prior art keywords
- solution
- carbonate
- cobalt
- manganese
- catalyst
- 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
- 239000003054 catalyst Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 12
- 230000003647 oxidation Effects 0.000 title claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 13
- 230000003472 neutralizing effect Effects 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 9
- 229910017052 cobalt Inorganic materials 0.000 claims description 8
- 239000010941 cobalt Substances 0.000 claims description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 8
- 239000011651 chromium Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 229910021446 cobalt carbonate Inorganic materials 0.000 claims description 6
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011656 manganese carbonate Substances 0.000 claims description 6
- 229940093474 manganese carbonate Drugs 0.000 claims description 6
- 235000006748 manganese carbonate Nutrition 0.000 claims description 6
- 229910001437 manganese ion Inorganic materials 0.000 claims description 6
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 6
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims description 3
- 238000010009 beating Methods 0.000 claims description 3
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 3
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 3
- 229910021645 metal ion Inorganic materials 0.000 claims description 3
- -1 metals ions Chemical class 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002910 solid waste Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 239000005711 Benzoic acid Substances 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical group [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Catalysts (AREA)
Abstract
The invention relates to the field of PTA production technology, and concretely relates to a method for reducing an oxidation catalyst in a PTA production apparatus. The catalyst in a waste liquid is recycled, HBr during the recovering process and Co<3+> produce Br<-> and Co<2+> which are catalyst compositions for dicarboxylic acid production, so as to re-perform an oxidation catalytic reaction.
Description
Technical field
The present invention relates to PTA production technology field, concretely, relate to reduce in a kind of PTA process units the method for oxidation catalyst.
Background technology
Contain benzoic acid, TA, Fe in the waste material of PTA production technology
3+, Cr
3+, Ni
2+, Co
3+, Mn
2+Plasma, Co in theory
2+Before and after reaction, do not change in composition, chemical property and quality before and after the reaction as catalyst, but in actual mechanical process, Co
2+Ion is along with the activity of carrying out of reaction reduces gradually and becomes Co
3+, Co
2+Cost higher, therefore be badly in need of a kind of technology and can recycle Co
2+Thereby, reduce the PTA production cost.
Summary of the invention
To above-mentioned technical problem, the present invention will provide the method for recycling oxidation catalyst in a kind of PTA process units.
Technical scheme to be solved by this invention is following:
Injecting water after joining in the recycling can to the solid slag powder in the residue evaporimeter pulls an oar; Solution after the making beating is delivered to flame filter press with pump; Contain metal ion and neutralizing tanks of a small amount of organic solution entering such as most cobalt, manganese, iron, nickel, chromium; PH through adding sodium carbonate liquor control neutralizing tank maintains between the 4-5; Corrosion metals ions such as the iron in the solution, nickel, chromium preferentially form carbonate deposition, and pass through a metal filtering core filter with these precipitate and separate; The solution such as a large amount of cobalt ions, manganese ion that contain after the separation get into another neutralizing tank; And add the sodium carbonate liquor prepared; Solution pH value in the neutralizing tank is controlled between the 8-9; Sodium carbonate can form carbonate deposition with cobalt, the manganese ion in the solution, and through the metal filtering core filter sediment is separated, and the cobalt carbonate after the separation, manganese carbonate sediment get in the dissolving tank subsequently; Addition through the control hydrobromic acid solution is with dissolving cobalt carbonate, manganese carbonate, and is deployed into the catalyst that oxidation reaction needs.
The invention has the advantages that: recycle the catalyst in the waste liquid, HBr in the removal process and cobalt and manganese form needed cobalt, manganese, the bromine catalyst of oxidation reaction again to be formed, and can carry out the oxidation catalysis reaction again.
The specific embodiment
Injecting water after being put into the solid waste in the residue evaporimeter in one recycling can pulls an oar; Solution after the making beating is delivered to flame filter press with pump; Contain metal ion and neutralizing tanks of a small amount of organic solution entering such as most cobalt, manganese, iron, nickel, chromium; PH through adding sodium carbonate liquor control neutralizing tank maintains between the 4-5; Corrosion metals ions such as the iron in the solution, nickel, chromium preferentially form carbonate deposition, and pass through a metal filtering core filter with these precipitate and separate; The solution such as a large amount of cobalt ions, manganese ion that contain after the separation get into another neutralizing tank; And add the sodium carbonate liquor prepared; Solution pH value in the neutralizing tank is controlled between the 8-9; Sodium carbonate can form carbonate deposition with cobalt, the manganese ion in the solution, and through the metal filtering core filter of two parallel connections sediment is separated, and the cobalt carbonate after the separation, manganese carbonate sediment get in the dissolving tank subsequently; Addition through the control hydrobromic acid solution is with dissolving cobalt carbonate, manganese carbonate, and is deployed into the catalyst that oxidation reaction needs.
Claims (1)
1. reduce the method for oxidation catalyst in the PTA process units; It is characterized in that: inject water after joining the solid waste in the residue evaporimeter in the recycling can and pull an oar; Solution after the making beating is delivered to flame filter press with pump; Contain metal ion and neutralizing tanks of a small amount of organic solution entering such as most cobalt, manganese, iron, nickel, chromium; PH through adding sodium carbonate liquor control neutralizing tank maintains between the 4-5, and corrosion metals ions such as the iron in the solution, nickel, chromium preferentially form carbonate deposition, and passes through a metal filtering core filter with these precipitate and separate; The solution such as a large amount of cobalt ions, manganese ion that contain after the separation get into another neutralizing tank; And add the sodium carbonate liquor prepared; Solution pH value in the neutralizing tank is controlled between the 8-9; Sodium carbonate can form carbonate deposition with cobalt, the manganese ion in the solution, and through the metal filtering core filter sediment is separated, and the cobalt carbonate after the separation, manganese carbonate sediment get in the dissolving tank subsequently; Addition through the control hydrobromic acid solution is with dissolving cobalt carbonate, manganese carbonate, and is deployed into the catalyst that oxidation reaction needs.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101586365A CN102824919A (en) | 2011-06-14 | 2011-06-14 | Method for reducing oxidation catalyst in PTA production apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101586365A CN102824919A (en) | 2011-06-14 | 2011-06-14 | Method for reducing oxidation catalyst in PTA production apparatus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102824919A true CN102824919A (en) | 2012-12-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101586365A Pending CN102824919A (en) | 2011-06-14 | 2011-06-14 | Method for reducing oxidation catalyst in PTA production apparatus |
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| CN (1) | CN102824919A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107597170A (en) * | 2017-10-28 | 2018-01-19 | 浙江上虞利星化工有限公司 | Method for preparing cobalt-manganese-bromine aqueous solution by utilizing recovered cobalt and manganese |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4410449A (en) * | 1979-12-14 | 1983-10-18 | Dynamit Nobel Aktiengesellschaft | Recovery and reuse of heavy-metal oxidation catalyst from the Witten DMT process |
| CN1293260A (en) * | 1999-10-19 | 2001-05-02 | 中国石化集团洛阳石油化工总厂 | Method for recovering cobalt and manganese catalyst in terephthalic acid oxidation residue |
| CN101259418A (en) * | 2008-04-15 | 2008-09-10 | 江苏大康实业有限公司 | Method for recovering and preparing cobalt-manganese catalyst from PTA oxidation residua beating wastewater |
-
2011
- 2011-06-14 CN CN2011101586365A patent/CN102824919A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4410449A (en) * | 1979-12-14 | 1983-10-18 | Dynamit Nobel Aktiengesellschaft | Recovery and reuse of heavy-metal oxidation catalyst from the Witten DMT process |
| CN1293260A (en) * | 1999-10-19 | 2001-05-02 | 中国石化集团洛阳石油化工总厂 | Method for recovering cobalt and manganese catalyst in terephthalic acid oxidation residue |
| CN101259418A (en) * | 2008-04-15 | 2008-09-10 | 江苏大康实业有限公司 | Method for recovering and preparing cobalt-manganese catalyst from PTA oxidation residua beating wastewater |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107597170A (en) * | 2017-10-28 | 2018-01-19 | 浙江上虞利星化工有限公司 | Method for preparing cobalt-manganese-bromine aqueous solution by utilizing recovered cobalt and manganese |
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Application publication date: 20121219 |