CN109776456A - A kind of starting method for establishing concentration gradient for realizing directly production ECH continuous production commercial run using phase transfer catalyst - Google Patents
A kind of starting method for establishing concentration gradient for realizing directly production ECH continuous production commercial run using phase transfer catalyst Download PDFInfo
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- CN109776456A CN109776456A CN201910142289.3A CN201910142289A CN109776456A CN 109776456 A CN109776456 A CN 109776456A CN 201910142289 A CN201910142289 A CN 201910142289A CN 109776456 A CN109776456 A CN 109776456A
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- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000010924 continuous production Methods 0.000 title claims abstract description 16
- 239000003444 phase transfer catalyst Substances 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 129
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000003054 catalyst Substances 0.000 claims abstract description 26
- OWXJKYNZGFSVRC-NSCUHMNNSA-N (e)-1-chloroprop-1-ene Chemical compound C\C=C\Cl OWXJKYNZGFSVRC-NSCUHMNNSA-N 0.000 claims abstract description 17
- 238000010992 reflux Methods 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000007791 liquid phase Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 5
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 4
- 229910001882 dioxygen Inorganic materials 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- -1 phospho Chemical group 0.000 claims description 3
- 238000005201 scrubbing Methods 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000005520 cutting process Methods 0.000 abstract 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 238000011084 recovery Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000013034 phenoxy resin Substances 0.000 description 1
- 229920006287 phenoxy resin Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Epoxy Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to epoxychloropropane production fields, and in particular to a kind of starting method for establishing concentration gradient that directly production ECH continuous production commercial run is realized using phase transfer catalyst, including chloropropene and catalyst are full of in reaction system in advance；Outlet and the entrance for cutting off reaction system, cut off the valve between reaction systems at different levels, make to form respective partial circulating inside reaction systems at different levels；Hydrogen peroxide is sequentially added by hand-operated valve on the tubular reactor of intergrade to first order reaction system, the H in intergrade tubular reactor2O2When lower than a certain value, normal production procedure is opened, so that each raw material is sequentially entered concatenated reaction system at different levels from pipeline and is reacted, guarantees that quantity-produced carries out.The present invention is ingenious in design, solve by normal production procedure can not deeper degree cause epoxychloropropane continuous production, the problem that feed stock conversion is low, product yield is low.The present invention is worth with market potential.
Description
Technical field
The present invention relates to epoxychloropropane production fields, and in particular to a kind of realized using phase transfer catalyst is directly produced
The starting method for establishing concentration gradient of ECH continuous production commercial run.
Background technique
Epoxychloropropane is a kind of organic compound, is mainly applicable to manufacture epoxy resin, it is also a kind of oxygen-containing
The stabilizer and chemical intermediate of substance, the primary raw material of epoxy group and phenoxy resin；It is also used for manufacture glycerol, curing propylene
Base rubber, the solvent of cellulose esters and ether, paper industry high wet-strength resins.The production method of epoxychloropropane has DECH at present
(direct oxidation) method, chlorohydrination, glycerol method and allyl acetate-allyl alcohol method, DECH method is due to great environment-friendly advantage, no waste residue, waste water
Amount is few, and has many advantages, such as that process is short, low energy consumption, is easy to enterprise's operation construction, gradually develops into epoxychloropropane production
The main direction of development of method.However DECH method is in laboratory stage Batch Process comparative maturity, and practical continuous production is run
In the process, quantity-produced method and apparatus, which is prepared, is but in the starting stage.
In quantity-produced start-up, it turns out that raw material, catalyst, auxiliary agent are by each according to conventional production procedure
From pipeline mix in a mixer after enter reaction of high order system reacted, cannot deeper degree initiation continuous production it is anti-
It answers, the extent of reaction is lower, and feed stock conversion and product yield are lower.
Summary of the invention
The technical problem to be solved by the present invention is to how to overcome the shortcomings of the prior art, provide a kind of using phase transfer
Catalyst realizes the starting method for establishing concentration gradient of directly production ECH continuous production commercial run.
The technical solution of the invention is as follows: a kind of realized using phase transfer catalyst directly produces ECH continuous production work
The starting method for establishing concentration gradient of industry method, comprising the following steps:
(1) after chloropropene mixes in material-compound tank with catalyst, concatenated reaction of high order system is flowed into, then from afterbody
Reaction system outflow returns to material-compound tank, makes in entire reaction system full of chloropropene and catalyst mixed liquid；(2) it closes and enters the
The chloropropene and catalyst mixed liquid pipeline valve of first order reaction system, close afterbody reaction system and the direct-connected pipe of material-compound tank
Valve on road closes the overflow tube valve being connected between reaction systems at different levels；(3) every order reaction system includes with cooling
The tubular reactor of system, the surge tank with the perforation connection of tubular reactor rear portion, the top of surge tank are logical equipped with nitrogen inlet
Enter nitrogen, the top perforation of surge tank is connected with condenser, and after surge tank gas phase enters condenser condensation, liquid-phase reflux enters buffering
Tank, gas phase enter scrubbing tower, and surge tank lower liquid phase reenters tubular reactor front by reflux pump reflux；(4) in opening
Hydrogen peroxide manually-operated gate on the tubular reactor of intercaste reaction system, is gradually added into hydrogen peroxide, until accumulation additional amount is to set
When definite value, stops hydrogen peroxide and be added；(5) dioxygen on the tubular reactor of intergrade reaction system previous stage reaction system is opened
Sailor's movable valve repeats step (4)；(6) step (5) are repeated forward, until opening the tubular reactor of first order reaction system
On hydrogen peroxide manually-operated gate, be gradually added into hydrogen peroxide, make accumulate additional amount setting value when, stop hydrogen peroxide addition；(7) exist
It is sampled in the tubular reactor of intergrade reaction system, works as H2O2Mass concentration be less than setting value when, opening steps are removed in (2)
All valves of valve on afterbody reaction system and the direct-connected pipeline of material-compound tank, into first order reaction system chloropropene,
Catalyst mixes in the mixer of front in tubular reactor after passing through reflux pump with from the hydrogen peroxide that dioxygen waterpipe enters,
It is reacted in tubular reactor again；The surge tank of overflow pipe connection two-stage reaction system, each order reaction between reaction systems at different levels
One by reflux pump reflux reenters tubular reactor to system buffer tank lower liquid phase, and another stock is entered next by overflow pipe
In order reaction system buffer tank；The valve on afterbody reaction system and separator pipeline is opened, afterbody is reacted
After the reaction product of system outflow enters separator separation, solid-phase catalyst reenters material-compound tank, and liquid phase enters rectifying system
System separation.
Further, catalyst is phospho heteropoly tungstate.
Further, the H in step (7)2O2Mass concentration setting value less than 0.8%.
Further, reaction of high order system is Pyatyi reaction system, and intergrade reaction system is third level reaction system.
The present invention produces the practical quantity-produced start-up of epoxychloropropane for chloropropene direct oxidation method, according to normal
The reaction process of rule, cannot good initiation reaction, the situation that feed stock conversion is low, product yield is low in reaction process carries out
It improves, chloropropene and catalyst is full of in reaction system by elder generation, then cut off the entrance and exit of reaction system, and each
Connection between order reaction system, then hydrogen peroxide is gradually respectively added in intergrade reaction system to first order reaction system, make
They carry out pre-reaction in respective reaction system, as the H of intergrade reaction system2O2Mass concentration be lower than by reaction
It when setting value, then opens normal production procedure and carries out successive reaction, by improving, stablize continuous production, feed stock conversion
High, product yield height, reaction time are shorter.The present invention is worth with market potential.
Detailed description of the invention
Fig. 1 is that chloropropene and catalyst are full of reaction system flow chart when driving in the present invention；
Fig. 2 is the normal continuous operation flow chart of the present invention.
Wherein, VE-1 is material-compound tank, and V-1 is the chloropropene and catalyst mixed liquid pipeline valve into first order reaction system
Door, PU-1 are first order reaction system flowback pump, and MX-1 is first order reaction system mixer, and RE-1 is that first order reaction system tubular type is anti-
Device is answered, V-8 is first order reaction system tubular reactor hydrogen peroxide manually-operated gate, and VE-2 is first order reaction system buffer tank, HE-1
For first order reaction system condenser, V-2 is first order reaction system and second order reaction system overflow tube valve, and V-3 is second order reaction
System and third-order reaction system overflow tube valve, PU-3 are third-order reaction system flowback pump, and MX-3 is the mixing of third-order reaction system
Device, RE-3 are third-order reaction system tubular reactor, and V-9 is third-order reaction system tubular reactor hydrogen peroxide manually-operated gate, VE-
4 be third-order reaction system buffer tank, and HE-3 is third-order reaction system condenser, and V-4 is third-order reaction system and fourth-order reaction system
System overflow tube valve, V-5 are fourth-order reaction system and Pyatyi reaction system overflow tube valve, and PU-5 is the reflux of Pyatyi reaction system
Pump, MX-5 are Pyatyi reaction system mixer, and RE-5 is Pyatyi reaction system tubular reactor, and VE-6 is slow for Pyatyi reaction system
Tank is rushed, HE-5 is Pyatyi reaction system condenser, and V-6 is Pyatyi reaction system and the direct-connected pipeline valve of material-compound tank, and V-7 Pyatyi is anti-
System and separator pipeline valve are answered, PU-2, PU-4 are second level, four reaction system reflux pumps, and RE-2, RE-4 are second level, four
Reaction system tubular reactor, VE-3, VE-5 are second level, four reaction system surge tanks, and HE-2, HE-4 are second level, four reaction systems
Unite condenser, two, fourth-order reaction system configuration it is identical as third-order reaction system, omit in the accompanying drawings.
Specific embodiment
With reference to embodiments and attached drawing, the present invention will be described in detail a kind of realizes directly production using phase transfer catalyst
The starting method for establishing concentration gradient of ECH continuous production commercial run.
It is a kind of to establish opening for concentration gradient using phase transfer catalyst realization directly production ECH continuous production commercial run
Vehicle method, comprising the following steps: as shown in Figure 1, flowing into series connection after (1) chloropropene mixes in material-compound tank VE-1 with catalyst
Reaction of high order system, then from afterbody Pyatyi reaction system flow out return material-compound tank VE-1, make to fill in entire reaction system
Full chloropropene and catalyst mixed liquid；(2) chloropropene and catalyst mixed liquid pipeline valve for entering first order reaction system are closed
Door V-1, closes the valve V-6 on afterbody Pyatyi reaction system and the direct-connected pipeline of material-compound tank VE-1, closes reaction systems at different levels
Overflow tube valve V-2, V-3, V-4, the V-5 being connected between system；(3) every order reaction system includes the tubular type with cooling system
Reactor RE-1, RE-2, RE-3, RE-4, RE-5 are penetrated through with the rear portion tubular reactor RE-1, RE-2, RE-3, RE-4, RE-5 and are connected
Surge tank VE-2, VE-3 for connecing, VE-4, VE-5, VE-6, the top of surge tank VE-2, VE-3, VE-4, VE-5, VE-6 are equipped with
Nitrogen inlet is passed through nitrogen, and the top perforation of surge tank VE-2, VE-3, VE-4, VE-5, VE-6 are connected with condenser HE-1, HE-
2, HE-3, HE-4, HE-5, surge tank VE-2, VE-3, VE-4, VE-5, VE-6 gas phase respectively enter condenser HE-1, HE-2,
After HE-3, HE-4, HE-5 condensation, liquid-phase reflux enters surge tank VE-2, VE-3, VE-4, VE-5, VE-6, and gas phase enters scrubbing tower,
Surge tank VE-2, VE-3, VE-4, VE-5, VE-6 lower liquid phase are flowed back heavy by reflux pump PU-1, PU-2, PU-3, PU-4, PU-5
Newly enter the front tubular reactor RE-1, RE-2, RE-3, RE-4, RE-5；(4) pipe of intergrade third level reaction system is opened
Hydrogen peroxide manually-operated gate V-9 on formula reactor RE-3, is gradually added into hydrogen peroxide, until stopping when accumulation additional amount is setting value
Only hydrogen peroxide is added；(5) it opens double on the tubular reactor RE-2 of intergrade reaction system previous stage second level reaction system
Oxygen sailor's movable valve repeats step (4)；(6) step (5) are repeated forward, until opening the pipe reaction of first order reaction system
Hydrogen peroxide manually-operated gate V-8 on device RE-1, is gradually added into hydrogen peroxide, when making to accumulate additional amount setting value, stops hydrogen peroxide
It is added；As shown in Fig. 2, (7) sample in the tubular reactor RE-3 of intergrade third level reaction system, work as H2O2Quality it is dense
When degree is less than setting value, except valve V-6 on afterbody reaction system and the direct-connected pipeline of material-compound tank VE-1 in opening steps (2)
All valves, into the chloropropene of first order reaction system, catalyst by entering after reflux pump PU-1 with from dioxygen waterpipe
Hydrogen peroxide mixed in the mixer MX-1 of front in tubular reactor RE-1, then reacted in tubular reactor RE-1；Respectively
Surge tank VE-2, VE-3, VE-4, VE-5, VE-6 of overflow pipe connection two-stage reaction system, each order reaction between order reaction system
System buffer tank VE-2, VE-3, VE-4, VE-5, VE-6 lower liquid phase one by reflux pump PU-1, PU-2, PU-3, PU-4, PU-
5 reflux reenter tubular reactor RE-1, RE-2, RE-3, RE-4, RE-5, and it is anti-that another stock by overflow pipe enters next stage
It answers in system buffer tank VE-3, VE-4, VE-5, VE-6；It opens on afterbody Pyatyi reaction system and separator pipeline
Valve V-7, after the reaction product for flowing out afterbody Pyatyi reaction system enters separator separation, solid-phase catalyst is again
Into material-compound tank VE-1, liquid phase enters distillation system separation.
Further, catalyst is phospho heteropoly tungstate.H in step (7)2O2Mass concentration setting value be less than
0.8%.
Such as table 1 is compared using starting method of the present invention and directly by every operating parameter that normal operation process is produced
It is shown.
The starting method of the present invention of table 1 and normal starting method parameter comparison
| Serial number | Starting method of the present invention | Positive starting method |
| It drives the time | 5~15h | 20~36h |
| H2O2Conversion ratio | 90~99% | 0~80% |
| Epoxychloropropane yield | 80~99% | 20~70% |
| Catalyst recovery yield | 90~99% | 0~60% |
As can be seen from Table 1, using starting method of the present invention, the time of driving is only 5~15h, so that it may reach normal
Production level, H2O2Conversion ratio, epoxychloropropane yield, catalyst recovery yield are higher, and normal production procedure is used to carry out
It drives, the time for reaching normal operation is longer, is 20~36h, energy consumption is high, and even if reaches normal operation, H2O2Conversion ratio,
Epoxychloropropane yield, catalyst recovery yield are also lower, in unstable, the halfway operating status of reaction.
Simply to illustrate that technical concepts and features of the invention, its purpose is allows in the art above-described embodiment
Those of ordinary skill cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all
It is the equivalent changes or modifications that the essence of content according to the present invention is made, should be covered by the scope of protection of the present invention.
Claims (4)
1. a kind of driving for establishing concentration gradient for realizing directly production ECH continuous production commercial run using phase transfer catalyst
Method, it is characterised in that the following steps are included:
(1) after chloropropene mixes in material-compound tank with catalyst, concatenated reaction of high order system is flowed into, then react from afterbody
System outflow returns to material-compound tank, makes in entire reaction system full of chloropropene and catalyst mixed liquid；
(2) chloropropene and catalyst mixed liquid pipeline valve for entering first order reaction system are closed, afterbody reaction is closed
Valve in system and the direct-connected pipeline of material-compound tank, closes the overflow tube valve being connected between reaction systems at different levels；
(3) every order reaction system includes the tubular reactor with cooling system, with the perforation connection of tubular reactor rear portion
Surge tank, the top of surge tank are equipped with nitrogen inlet and are passed through nitrogen, and the top perforation of surge tank is connected with condenser, surge tank gas
After mutually entering condenser condensation, liquid-phase reflux enters surge tank, and gas phase enters scrubbing tower, and surge tank lower liquid phase is by reflux pump reflux
Reenter tubular reactor front；
(4) the hydrogen peroxide manually-operated gate on the tubular reactor of intergrade reaction system is opened, hydrogen peroxide is gradually added into, until tired
When product additional amount is setting value, stops hydrogen peroxide and be added；
(5) the hydrogen peroxide manually-operated gate on the tubular reactor of intergrade reaction system previous stage reaction system is opened, repeats to walk
Suddenly (4)；
(6) step (5) are repeated forward, until the hydrogen peroxide manually-operated gate on the tubular reactor of first order reaction system is opened,
It is gradually added into hydrogen peroxide, when making to accumulate additional amount setting value, stops hydrogen peroxide and is added；
(7) it is sampled in the tubular reactor of intergrade reaction system, works as H2O2Mass concentration be less than setting value when, open step
Suddenly except all valves of valve on afterbody reaction system and the direct-connected pipeline of material-compound tank in (2), into first order reaction system
Chloropropene, catalyst by after reflux pump with the mixing from hydrogen peroxide front in tubular reactor that dioxygen waterpipe enters
It mixes in device, then is reacted in tubular reactor；The surge tank of overflow pipe connection two-stage reaction system between reaction systems at different levels,
One by reflux pump reflux reenters tubular reactor to reaction system surge tank lower liquid phases at different levels, and another stock passes through overflow pipe
Into in next stage reaction system surge tank；The valve on afterbody reaction system and separator pipeline is opened, is made last
After the reaction product of first order reaction system outflow enters separator separation, solid-phase catalyst reenters material-compound tank, liquid phase into
Enter distillation system separation.
2. a kind of realized using phase transfer catalyst according to claim 1 directly produces ECH continuous production commercial run
The starting method for establishing concentration gradient, it is characterised in that: catalyst is phospho heteropoly tungstate.
3. a kind of realized using phase transfer catalyst according to claim 1 directly produces ECH continuous production commercial run
The starting method for establishing concentration gradient, it is characterised in that: the H in step (7)2O2Mass concentration setting value less than 0.8%.
4. a kind of realized using phase transfer catalyst according to claim 1 directly produces ECH continuous production commercial run
The starting method for establishing concentration gradient, it is characterised in that: reaction of high order system be Pyatyi reaction system, intergrade reaction system
For third level reaction system.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204512A (en) * | 2019-06-04 | 2019-09-06 | 山东凯泰科技股份有限公司 | A kind of technique using phase transfer catalyst direct oxidation production epoxychloropropane |
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| CN109776456B (en) | 2022-04-15 |
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