CN204039305U - A kind of production unit of oxidation inhibitor - Google Patents
A kind of production unit of oxidation inhibitor Download PDFInfo
- Publication number
- CN204039305U CN204039305U CN201420367454.8U CN201420367454U CN204039305U CN 204039305 U CN204039305 U CN 204039305U CN 201420367454 U CN201420367454 U CN 201420367454U CN 204039305 U CN204039305 U CN 204039305U
- Authority
- CN
- China
- Prior art keywords
- reaction still
- oxidation inhibitor
- kettle
- production unit
- utility
- 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.)
- Expired - Lifetime
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 239000003112 inhibitor Substances 0.000 title claims abstract description 17
- 230000003647 oxidation Effects 0.000 title claims abstract description 17
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000002425 crystallisation Methods 0.000 claims abstract description 20
- 230000008025 crystallization Effects 0.000 claims abstract description 20
- 238000003747 Grignard reaction Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 239000006200 vaporizer Substances 0.000 claims description 5
- 150000002901 organomagnesium compounds Chemical class 0.000 abstract description 9
- 239000002904 solvent Substances 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 235000021050 feed intake Nutrition 0.000 abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 4
- -1 polypropylene Polymers 0.000 description 4
- 238000001953 recrystallisation Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- HQJQYILBCQPYBI-UHFFFAOYSA-N 1-bromo-4-(4-bromophenyl)benzene Chemical group C1=CC(Br)=CC=C1C1=CC=C(Br)C=C1 HQJQYILBCQPYBI-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- ZFJMTDFOGDGPTF-UHFFFAOYSA-N phosphanium;chloride;hydrochloride Chemical compound P.Cl.Cl ZFJMTDFOGDGPTF-UHFFFAOYSA-N 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 238000005727 Friedel-Crafts reaction Methods 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000008301 phosphite esters Chemical class 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Abstract
The utility model discloses a kind of production unit of oxidation inhibitor, for the manufacture field of oxidation inhibitor, comprise grignard reaction still, low-temp reaction still, washing kettle and crystallization kettle, described grignard reaction still, low-temp reaction still, washing kettle are connected by pipeline successively with crystallization kettle.The each reaction unit of the utility model connects simple, feed intake easy to control, easy to operate and safe, reaction process is gentle, can realize preparation four (2,4-di-tert-butyl-phenyl)-4, the new technology of 4 '-xenyl bis-phosphite, compared with prior art, catalyst selectivity is good, and product yield is high.Washing kettle eliminates the unstable of organo-magnesium compound solution, guarantees the security of producing.Reaction process is gentle, and equipment is not easily corroded.Produce solvent used recyclable, environmental protection.
Description
Technical field
The utility model is used for the manufacture field of oxidation inhibitor, particularly relates to a kind of production unit of oxidation inhibitor.
Background technology
Four (2,4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite is a kind of phosphite ester kind antioxidant.It has excellent heat resistant and anti-hydrolytic performance, therefore can be used as auxiliary antioxidant and is widely used in the many general plastics such as polypropylene, polyethylene, ABS resin, polycarbonate and engineering plastics.Domestic literature report four (2,4-di-tert-butyl-phenyl)-4, the synthesis of 4 '-xenyl bis-phosphite is with biphenyl, phosphorus trichloride and aluminum trichloride (anhydrous) for main raw material, prepares intermediate 4 under certain condition by Friedel-Crafts reaction, the complex compound of the two dichloride phosphine of 4 '-xenyl.By adding the decomplexing agent of phosphorus oxychloride or pyridine etc., obtain intermediate 4, the two dichloride phosphine of 4 '-xenyl.Finally, intermediate prepares phosphite antioxidant four (2,4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite by esterification.Its production process uses a large amount of solid catalysts of being fuming, and causes heavy corrosion to equipment.And produce expendable waste residue of being fuming in a large number, serious impact is caused on ecotope.
In order to overcome the deficiency of existing production technology, the present inventor to set out preparation four (2,4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite from 4,4-'-dibromobiphenyl.As compared to the technology of preparation four (2,4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite of domestic report, employ the iodine catalyst of stable in properties, addition is few, and catalyst selectivity is good, and product yield is high.Reaction process is gentle, and equipment is not easily corroded.
Utility model content
For implementing the new technology of above-mentioned preparation four (2,4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite, the utility model provides a kind of and connects simply, feeds intake easy to control, easy to operate and safe, the production unit of the oxidation inhibitor of reaction process gentleness.
The utility model solves the technical scheme that its technical problem adopts: a kind of production unit of oxidation inhibitor, comprise grignard reaction still, low-temp reaction still, washing kettle and crystallization kettle, described grignard reaction still, low-temp reaction still, washing kettle are connected by pipeline successively with crystallization kettle.
Be further used as the improvement of technical solutions of the utility model, the pipeline between described grignard reaction still and low-temp reaction still is provided with the first strainer.
Be further used as the improvement of technical solutions of the utility model, the pipeline between described washing kettle and crystallization kettle is provided with the second strainer.
Be further used as the improvement of technical solutions of the utility model, the pipeline between described second strainer and crystallization kettle is provided with vaporizer.
Be further used as the improvement of technical solutions of the utility model, also comprise moisture eliminator, described moisture eliminator is connected with described crystallization kettle by pipeline.
Be further used as the improvement of technical solutions of the utility model, the pipeline between described crystallization kettle and moisture eliminator is provided with whizzer.
The beneficial effects of the utility model: the utility model is in production four (2,4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite time, by 4 in grignard reaction still, 4-'-dibromobiphenyl, magnesium chips, solvent, by grignard reaction, generate the organo-magnesium compound solution containing solvent; Organo-magnesium compound solution is entered in low-temp reaction still by pipeline, and reacts at low temperatures with two (2,4-di-tert-butyl-phenyl) sub-phosphoryl chloride solution and generate oxidation inhibitor four (2,4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite; Organo-magnesium compound residual in low-temp reaction still is entered washing kettle by pipeline, and with the reaction such as water, weak base, generate stable molecule, its high reactivity be damaged; Then enter crystallization kettle by pipeline, in crystallization kettle, add the solid recrystallization that methyl alcohol or Virahol will be wet.
The each reaction unit of the utility model connects simple, feed intake easy to control, easy to operate and safe, reaction process is gentle, can realize preparation four (2,4-di-tert-butyl-phenyl)-4, the new technology of 4 '-xenyl bis-phosphite, compared with prior art, catalyst selectivity is good, and product yield is high.Washing kettle eliminates the unstable of organo-magnesium compound solution, guarantees the security of producing.Reaction process is gentle, and equipment is not easily corroded.Produce solvent used recyclable, environmental protection.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the utility model is described in further detail:
Fig. 1 is the utility model example structure schematic diagram.
Embodiment
With reference to Fig. 1, the utility model provides a kind of oxidation inhibitor, and (present embodiment is with four (2,4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite is example) production unit, comprise grignard reaction still 1, first strainer 2, low-temp reaction still 3, washing kettle 4, second strainer 5, vaporizer 6, crystallization kettle 7, whizzer 8 and moisture eliminator 9, grignard reaction still 1, first strainer 2, low-temp reaction still 3, washing kettle 4, second strainer 5, vaporizer 6, crystallization kettle 7, whizzer 8 and moisture eliminator 9 connect into entirety by pipeline successively, realize flowing water work.
In described grignard reaction still 1,4,4-'-dibromobiphenyl, magnesium chips, solvent are passed through grignard reaction, generate the organo-magnesium compound solution containing solvent.Grignard reaction still 1 kettle cover has charging opening, nitrogen inlet, reflux inlet etc.React complete first strainer 2 that enters after cooling by the magnesium chips elimination of remainder.
In described low-temp reaction still 3, organo-magnesium compound solution is reacted at low temperatures with two (2,4-di-tert-butyl-phenyl) sub-phosphoryl chloride solution and generate oxidation inhibitor four (2,4-di-tert-butyl-phenyl)-4,4 '-xenyl bis-phosphite.
Described washing kettle 4 be by organo-magnesium compound residual in low-temp reaction still by with the reaction such as water, weak base, generate stable molecule, its high reactivity be damaged.Water layer is separated with oil reservoir, and water-fast impurity enters the second strainer filter 5 and goes.Then clean oil reservoir enters recycling design in vaporizer 6, and the solid obtaining wetting enters crystallization kettle 7.
Described crystallization kettle 7 adds the solid recrystallization that methyl alcohol or Virahol will be wet.After recrystallization, solution enters whizzer 8 by solid and separated from solvent, and the wet solid after recrystallization enters moisture eliminator 9 thoroughly except desolventizing and micro-moisture.
The each reaction unit of the utility model connects simple, feed intake easy to control, easy to operate and safe, reaction process is gentle, can realize preparation four (2,4-di-tert-butyl-phenyl)-4, the new technology of 4 '-xenyl bis-phosphite, compared with prior art, catalyst selectivity is good, and product yield is high.Washing kettle 4 eliminates the unstable of organo-magnesium compound solution, guarantees the security of producing.Reaction process is gentle, and equipment is not easily corroded.Produce solvent used recyclable, environmental protection.
Certainly, the invention is not limited to above-mentioned embodiment, those of ordinary skill in the art also can make equivalent variations or replacement under the prerequisite without prejudice to the utility model spirit, and these equivalent modification or replacement are all included in the application's claim limited range.
Claims (6)
1. a production unit for oxidation inhibitor, is characterized in that: comprise grignard reaction still, low-temp reaction still, washing kettle and crystallization kettle, and described grignard reaction still, low-temp reaction still, washing kettle are connected by pipeline successively with crystallization kettle.
2. the production unit of oxidation inhibitor according to claim 1, is characterized in that: the pipeline between described grignard reaction still and low-temp reaction still is provided with the first strainer.
3. the production unit of oxidation inhibitor according to claim 1 and 2, is characterized in that: the pipeline between described washing kettle and crystallization kettle is provided with the second strainer.
4. the production unit of oxidation inhibitor according to claim 3, is characterized in that: the pipeline between described second strainer and crystallization kettle is provided with vaporizer.
5. the production unit of oxidation inhibitor according to claim 4, is characterized in that: also comprise moisture eliminator, described moisture eliminator is connected with described crystallization kettle by pipeline.
6. the production unit of oxidation inhibitor according to claim 5, is characterized in that: the pipeline between described crystallization kettle and moisture eliminator is provided with whizzer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420367454.8U CN204039305U (en) | 2014-07-04 | 2014-07-04 | A kind of production unit of oxidation inhibitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420367454.8U CN204039305U (en) | 2014-07-04 | 2014-07-04 | A kind of production unit of oxidation inhibitor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN204039305U true CN204039305U (en) | 2014-12-24 |
Family
ID=52239996
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201420367454.8U Expired - Lifetime CN204039305U (en) | 2014-07-04 | 2014-07-04 | A kind of production unit of oxidation inhibitor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN204039305U (en) |
-
2014
- 2014-07-04 CN CN201420367454.8U patent/CN204039305U/en not_active Expired - Lifetime
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20141224 |