CN202185160U - A retrieve methyl alcohol stills for preparing calcium acetylacetonate - Google Patents
A retrieve methyl alcohol stills for preparing calcium acetylacetonate Download PDFInfo
- Publication number
- CN202185160U CN202185160U CN2011202618123U CN201120261812U CN202185160U CN 202185160 U CN202185160 U CN 202185160U CN 2011202618123 U CN2011202618123 U CN 2011202618123U CN 201120261812 U CN201120261812 U CN 201120261812U CN 202185160 U CN202185160 U CN 202185160U
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- Prior art keywords
- steam
- distillation still
- pipe
- methyl alcohol
- water
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 106
- QAZYYQMPRQKMAC-FDGPNNRMSA-L calcium;(z)-4-oxopent-2-en-2-olate Chemical compound [Ca+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O QAZYYQMPRQKMAC-FDGPNNRMSA-L 0.000 title claims abstract description 22
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000004821 distillation Methods 0.000 claims abstract description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000011084 recovery Methods 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000007599 discharging Methods 0.000 abstract 3
- 238000010923 batch production Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- IEDKVDCIEARIIU-UHFFFAOYSA-N 2-Nonadecanone Chemical compound CCCCCCCCCCCCCCCCCC(C)=O IEDKVDCIEARIIU-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- DFADSEMLTJRBFX-UHFFFAOYSA-N calcium;pentane-2,4-dione Chemical compound [Ca].CC(=O)CC(C)=O DFADSEMLTJRBFX-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- NZZIMKJIVMHWJC-UHFFFAOYSA-N dibenzoylmethane Chemical compound C=1C=CC=CC=1C(=O)CC(=O)C1=CC=CC=C1 NZZIMKJIVMHWJC-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model aims at providing a recovery methyl alcohol stills structure for preparing calcium acetylacetonate for batch production. A methanol recovery distillation still structure for preparing calcium acetylacetonate comprises a distillation still; a steam cavity is attached to the outside of the distillation kettle, the top of the distillation kettle is provided with a methanol, a small amount of water and a small amount of acetylacetone feeding pipe and a methanol and water steam discharging pipe, the bottom of the distillation kettle is provided with a drain pipe, and the steam cavity is provided with a steam inlet pipe and a steam outlet pipe; the distillation kettle is elliptical; the steam cavity extends from the upper part of the distillation kettle to the bottom of the distillation kettle; the steam inlet pipe is positioned at the upper part of the steam cavity, and the steam outlet pipe is positioned at the lower part of the steam cavity; a thermometer and a pressure gauge are arranged at the top of the distillation still; the methanol, a small amount of water and a small amount of acetylacetone feeding pipe, the methanol and water steam discharging pipe, the blow-off pipe, the steam inlet pipe and the steam outlet pipe are all provided with ball valves. Distilling and recovering methanol for preparing calcium acetylacetonate in the distillation still, and discharging impurities.
Description
Technical field
The utility model relates to the preparation calcium acetylacetonate, relates in particular to a kind of recovery methyl alcohol distillation still structure that is used to prepare calcium acetylacetonate.
Background technology
Synthesizing of acetylacetonate, more existing reports, liquid phase method is in the majority, and solid phase method occurs in recent years on a small quantity.Of many uses through the market survey calcium acetylacetonate, it can be used as halide heat stabilizers such as hard PVC, with stearoyl methane, dibenzoyl methane significant synergy is arranged.It also can be used as the promoter of hardening of resin, resin cross-linking agent, the additive of resin, rubber, the formation agent of ultra conducting membranes, hotline-reflective glass, nesa coating.
In traditional liquid phase method synthesis of acetyl acetone calcium technology, in calcium chloride solution, add NaOH earlier, angry calcium hydroxide adds the acetylacetone,2,4-pentanedione reaction again and generates calcium acetylacetonate.Owing in the aqueous solution, react, acetylacetone,2,4-pentanedione has the part decomposition loss, and the separation of liquid phase method needs the labor energy in addition.Experiment finds to adopt this legal system to get calcium acetylacetonate, and the reaction time is long, and efficiency of pcr product is not high, detects product with ultraviolet spectrophotometry, and absworption peak is more, explains that accessory substance is many.Solid phase method is the near research focus that comes the acetylacetonate synthetic method, and this method directly is that raw material and acetylacetone,2,4-pentanedione reacting by heating generate calcium acetylacetonate with calcium hydroxide.This method mild condition, simple to operate, reaction speed is fast, high selectivity, high yield, and low energy consumption, environmental friendliness have universal applicability, have also avoided the harmful effect to functional mixture simultaneously.Be retarder thinner with methyl alcohol when selecting solid phase method for use, both helped operation and reaction and carried out, help the recovery of reactant and the washing and the recovery of product again through experiment showed.
Yet existing theory does not all relate to the equipment that processing step is adopted when producing in batches.
The utility model content
The purpose of the utility model is for producing calcium acetylacetonate in batches a kind of recovery methyl alcohol distillation still structure that is used to prepare calcium acetylacetonate to be provided.
The above-mentioned technical purpose of the utility model is achieved through following technical scheme:
A kind of recovery methyl alcohol distillation still structure that is used to prepare calcium acetylacetonate, it comprises distillation still; Distillation still is outward with vapor chamber, and the distillation still top is provided with the steam discharge nozzle of methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione feed pipe and first alcohol and water, and the distillation still bottom is provided with blow-off pipe, and vapor chamber is provided with steam inlet tube and steam goes out pipe.
Preferred as technique scheme, said distillation still is ellipticity.
Preferred as technique scheme, said vapor chamber extends to the distillation still bottom from distillation still top.
Preferred as technique scheme, said steam inlet tube is positioned at the top of vapor chamber, and said steam goes out the bottom that pipe is positioned at vapor chamber.
Preferred as technique scheme, said distillation still top is provided with thermometer and pressure gauge.
Preferred as technique scheme, steam discharge nozzle, blow-off pipe, steam inlet tube and the steam of said methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione feed pipe, first alcohol and water go out on the pipe all to be provided with ball valve.
Open the ball valve on methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione feed pipe; Methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione are sent into distillation still; Open distillation still and stir, the ball valve of opening on the steam inlet tube is sent steam into vapor chamber, and material in the distillation still is added thermal distillation; Open steam simultaneously and go out the ball valve on the pipe; The recovered steam lime set is opened the ball valve on the steam discharge nozzle of first alcohol and water, the methanol gas that distillation produces and water vapour next step recovery process of steam discharge nozzle entering through the first alcohol and water.Treat cooling in the still after distillation is accomplished, open the ball valve on the blow-off pipe, carry out blowdown.Through thermometer and pressure gauge control distillation temperature in the kettle and pressure.
In sum; The utlity model has following beneficial effect: methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione are sent into distillation still from methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione feed pipe; The methyl alcohol of in distillation still, the preparation calcium acetylacetonate being used distills recovery, discharges impurity.
Description of drawings
Fig. 1 is a distillation still sectional structure sketch map;
1-distillation still among the figure, the 2-vapor chamber, 11-methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione feed pipe, the steam discharge nozzle of 12-first alcohol and water, the 13-blow-off pipe, the 14-thermometer, the 15-pressure gauge, the 21-steam inlet tube, 22-steam goes out pipe, 111-ball valve.
The specific embodiment
Below in conjunction with accompanying drawing the utility model is done further explain.
This specific embodiment only is the explanation to the utility model; It is not the restriction to the utility model; Those skilled in the art can make the modification that does not have creative contribution to present embodiment as required after reading this specification, but as long as in the claim scope of the utility model, all receive the protection of Patent Law.
A kind of recovery methyl alcohol distillation still structure that is used to prepare calcium acetylacetonate shown in accompanying drawing, it comprises distillation still 1; Distillation still 1 is outer with vapor chamber 2, and distillation still 1 top is provided with the steam discharge nozzle 12 of methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione feed pipe 11 and first alcohol and water, and distillation still 1 bottom is provided with blow-off pipe 13, and vapor chamber 2 is provided with steam inlet tube 21 and goes out pipe 22 with steam; Distillation still 1 is ellipticity; Vapor chamber 2 extends to distillation still 1 bottom from distillation still 1 top; Steam inlet tube 21 is positioned at the top of vapor chamber 2, and steam goes out the bottom that pipe 22 is positioned at vapor chamber 2; Distillation still 1 top is provided with thermometer 14 and pressure gauge 15; Steam discharge nozzle 12, blow-off pipe 13, steam inlet tube 21 and the steam of methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione feed pipe 11, first alcohol and water go out on the pipe 22 all to be provided with ball valve 111.
Open the ball valve 111 of methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione feed pipe 11; Methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione are sent into distillation still 1; Open distillation still 1 and stir, the ball valve of opening on the steam inlet tube 21 111 is sent steam into vapor chamber 2, and material in the distillation still 1 is added thermal distillation; Open steam simultaneously and go out the ball valve on the pipe 22; The recovered steam lime set is opened the ball valve 111 on the steam discharge nozzle 12 of first alcohol and water, the methanol gas that distillation produces and water vapour steam discharge nozzle 12 next step recovery process of entering through the first alcohol and water.Treat cooling in the still after distillation is accomplished, open the ball valve 111 on the blow-off pipe 13, carry out blowdown.Through thermometer 14 and pressure gauge 15 control distillation temperature in the kettle and pressure.
Claims (6)
1. recovery methyl alcohol distillation still structure that is used to prepare calcium acetylacetonate, it is characterized in that: it comprises distillation still (1); Distillation still (1) is outer with vapor chamber (2); Distillation still (1) top is provided with the steam discharge nozzle (12) of methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione feed pipe (11) and first alcohol and water; Distillation still (1) bottom is provided with blow-off pipe (13), and vapor chamber (2) is provided with steam inlet tube (21) and steam goes out pipe (22).
2. according to the said a kind of recovery methyl alcohol distillation still structure that is used to prepare calcium acetylacetonate of claim 1, it is characterized in that: said distillation still (1) is ellipticity.
3. according to the said a kind of recovery methyl alcohol distillation still structure that is used to prepare calcium acetylacetonate of claim 2, it is characterized in that: said vapor chamber (2) extends to distillation still (1) bottom from distillation still (1) top.
4. according to the said a kind of recovery methyl alcohol distillation still structure that is used to prepare calcium acetylacetonate of claim 3, it is characterized in that: said steam inlet tube (21) is positioned at the top of vapor chamber (2), and said steam goes out the bottom that pipe (22) is positioned at vapor chamber (2).
5. according to the said a kind of recovery methyl alcohol distillation still structure that is used to prepare calcium acetylacetonate of claim 4, it is characterized in that: said distillation still (1) top is provided with thermometer (14) and pressure gauge (15).
6. according to the said a kind of recovery methyl alcohol distillation still structure that is used to prepare calcium acetylacetonate of claim 5, it is characterized in that: steam discharge nozzle (12), blow-off pipe (13), steam inlet tube (21) and the steam of said methyl alcohol, low amounts of water and a small amount of acetylacetone,2,4-pentanedione feed pipe (11), first alcohol and water go out on the pipe (22) all to be provided with ball valve (111).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202618123U CN202185160U (en) | 2011-07-22 | 2011-07-22 | A retrieve methyl alcohol stills for preparing calcium acetylacetonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202618123U CN202185160U (en) | 2011-07-22 | 2011-07-22 | A retrieve methyl alcohol stills for preparing calcium acetylacetonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202185160U true CN202185160U (en) | 2012-04-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011202618123U Expired - Fee Related CN202185160U (en) | 2011-07-22 | 2011-07-22 | A retrieve methyl alcohol stills for preparing calcium acetylacetonate |
Country Status (1)
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| CN (1) | CN202185160U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110227278A (en) * | 2019-07-22 | 2019-09-13 | 余小海 | A kind of toluene distillation kettle |
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2011
- 2011-07-22 CN CN2011202618123U patent/CN202185160U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110227278A (en) * | 2019-07-22 | 2019-09-13 | 余小海 | A kind of toluene distillation kettle |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120411 Termination date: 20140722 |
|
| EXPY | Termination of patent right or utility model |