CN109776424A - A kind of MIC reactor prepares the new method of L-Phenylglycine precursor benzene glycolylurea - Google Patents
A kind of MIC reactor prepares the new method of L-Phenylglycine precursor benzene glycolylurea Download PDFInfo
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Abstract
The present invention relates to the new methods that a kind of MIC reactor prepares L-Phenylglycine precursor benzene glycolylurea.Prior art uses reaction kettle batch production, and disordered exhaust gas is more, and it is possible to turn to expect that there are sealing surface material leakage in the process, and security risk and environmentally friendly risk are all higher.Ammonium hydrogen carbonate (pure), Cymag (30% aqueous solution) and benzaldehyde are pumped into have been warmed up by the present invention with the mass ratio of 8.2:15.8:10 carries out hybrid reaction into 60 DEG C of MIC reactor, preparation solution hydrolyzes to obtain mixed phenylglycine, the MIC reactor discharge port connects knockout drum, the gas vent of knockout drum connects pressure gauge and shows that system pressure, knockout drum are further connected with counterbalance valve and carry out back pressure to whole system.The present invention substitutes solid ammonium bicarbonate using ammonium bicarbonate aqueous solution, has successfully evaded the dust and disordered exhaust gas generated when solid ammonium bicarbonate feeds intake, in addition the dosage of ammonium hydrogen carbonate drops to 1.1 equivalents by 1.5 equivalents, and economic benefit is obvious.
Description
Technical field
The present invention relates to the new methods that a kind of MIC reactor prepares L-Phenylglycine precursor benzene glycolylurea.
Background technique
Manufacturer all produces L-Phenylglycine using Bucherer-Bergs method substantially both at home and abroad at present, and the method is with benzene
Formaldehyde is starting material, and benzene glycolylurea is made with excessive ammonium hydrogen carbonate (or ammonium carbonate) under Cymag (or potassium cyanide) effect,
Hydrolyzed again, split obtained L-Phenylglycine, benzene glycolylurea yield (in terms of benzaldehyde) 80% or so, wastewater treatment difficulty compared with
Greatly.
Bucherer-Bergs method uses a large amount of extremely toxic substance Cymags (or potassium cyanide), has a small amount of cyaniding hydrogen in reaction
Body generates, and there are CN- in reaction solution, has higher want to equipment safety operation, occupational health control measure, environment protection treating facility
It asks.In addition, the technique uses reaction kettle batch production, disordered exhaust gas is more, and turning material, there are sealing surface material leakage in the process
May, security risk and environmentally friendly risk are all higher.
Summary of the invention
In view of the problems of the existing technology the present invention, provides a kind of MIC reactor and prepares L-Phenylglycine precursor benzene
The new method of glycolylurea, the present invention using continuous and automatic production technique substitute batch production technique, reduce to the greatest extent material with
Extraneous contact frequency reduces the generation of exhaust gas, also reduces production cost.
The technical solution adopted by the present invention is that: a kind of MIC reactor prepares the new side of L-Phenylglycine precursor benzene glycolylurea
Method, it is characterised in that by ammonium hydrogen carbonate (pure), Cymag (30% aqueous solution) and benzaldehyde with the mass ratio of 8.2:15.8:10
Example, which is pumped into have been warmed up into 60 DEG C of MIC reactor, carries out hybrid reaction, and preparation solution hydrolyzes to obtain mixed phenylglycine, described
MIC reactor discharge port connects knockout drum, and the gas vent of knockout drum connects pressure gauge and shows system pressure, gas-liquid separation
Tank is further connected with counterbalance valve and carries out back pressure to whole system.It is pumped into have been warmed up and carries out hybrid reaction into 60 DEG C of MIC reactor,
Preparation solution hydrolyzes to obtain mixed phenylglycine, and the MIC reactor discharge port connects knockout drum, and the gas of knockout drum goes out
Mouth connects pressure gauge and shows that system pressure, knockout drum are further connected with counterbalance valve and carry out back pressure to whole system.The present invention passes through liquid
Mixed phenylglycine is made in basic hydrolysis, then splits through d-camphorsulfonic acid and L-Phenylglycine is made, and is ampicillin, cephalo
The semi-synthetic important intermediate of ammonia benzyl and other beta-lactam antibiotics.MIC reactor heat buffering of the present invention needs
The amount of asking is low, and the degree of automation is high, meets clean manufacturing requirement, represents the developing direction of Green Chemistry and automation.
The ammonium bicarbonate aqueous solution for accounting for its gross mass 60% is first pumped into when preparation, then flow set pumps three raw materials simultaneously
It is complete.
When preparation respectively by ammonium bicarbonate aqueous solution, 30% Cymag, benzaldehyde respectively with 2800L/h, 940L/h,
The flow of 600L/h is continuously pumped into MIC reactor.
The MIC inside reactor is inserted into 2205 stainless steel microchannel inserted sheet of nanoscale.Reinforce benzaldehyde and 30% cyanogen
Change shear action when sodium mixing, strengthens mixed process
The MIC inside reactor channel arranged in parallel, single channel size are constant.Slow down Bucherer-Bergs
The enlarge-effect of reaction process.
The beneficial effects of the present invention are: it can be realized " closure production technology substitutes open type production technology " and " connect
The environmental protection policies requirements such as continuousization, automatic production process substitution batch production technique ", while MIC reactor preparation method category
In " micro- reaction, continuous flow " scope, meet current safety policy requirements.
The present invention substitutes solid ammonium bicarbonate using ammonium bicarbonate aqueous solution, when successfully having evaded solid ammonium bicarbonate and feeding intake
The dust and disordered exhaust gas of generation, in addition the dosage of ammonium hydrogen carbonate drops to 1.1 equivalents by 1.5 equivalents, and economic benefit is obvious.
The most key, using the preparation method of MIC reactor, benzene glycolylurea (in terms of benzaldehyde) yield can be improved by existing 80%
To 92%, 12% is improved, remarkable in economical benefits.
Detailed description of the invention
Fig. 1 is synthetic route schematic diagram of the invention.
The position Fig. 2 reaction mechanism schematic diagram of the invention.
The structural schematic diagram of the position Fig. 3 MIC reactor of the invention.
Specific embodiment
With reference to the accompanying drawing, of the invention is described in detail:
As shown in Figure 1-3, MIC reactor discharge port connects knockout drum, the gas vent of knockout drum connects pressure gauge
Show that system pressure, knockout drum are further connected with counterbalance valve and carry out back pressure to whole system.MIC inside reactor is inserted into nanoscale
2205 stainless steel microchannel inserted sheets.MIC inside reactor channel arranged in parallel, single channel size are constant.Specific preparation method
It is as follows:
Embodiment 1: by 820kg ammonium hydrogen carbonate (pure), 1580kg Cymag (30% aqueous solution), 1000kg benzaldehyde point
It is not pumped into the MIC reactor having been warmed up to 60 DEG C from MIC Reactor inlet by metering pump, notices that ammonium bicarbonate aqueous solution first pumps
Enter about 500kg, then be pumped into benzaldehyde, ammonium bicarbonate aqueous solution and 30% Cymag simultaneously, flow set with three raw materials simultaneously
Subject to having pumped.Preparation solution hydrolyzes to obtain 1644kg mixed phenylglycine, testing result are as follows: loss on drying: 19.23%；Sulfate radical:
2ppm；Alkali light absorption value: 0.277AU.
Embodiment 2:
Ammonium bicarbonate aqueous solution, 30% Cymag, benzaldehyde are connected respectively with the flow of 2800L/h, 940L/h, 600L/h
Continue and be pumped into the MIC reactor for being pre-heated to 60 DEG C, satisfactory preparation solution can be continuously available, it is qualified that preparation solution can be obtained through hydrolysis
Mixed phenylglycine.Pay attention to wanting whether moment attentive response liquid becomes blue in continuous preparation process, if becoming blue, illustrates reaction system
Middle Cymag is excessive, need to reduce the inlet amount of 30% Cymag in time.
It is sub that the above enumerated are only specific embodiments of the present invention, and the present invention is not limited to the above embodiments, can also have
Many deformations.All deformations that those skilled in the art directly can export or associate from present disclosure,
It is considered as protection scope of the present invention.
Claims (5)
1. the new method that a kind of MIC reactor prepares L-Phenylglycine precursor benzene glycolylurea, it is characterised in that by ammonium hydrogen carbonate (folding
It is pure), Cymag (30% aqueous solution) and benzaldehyde the MIC having been warmed up to 60 DEG C is pumped into the mass ratio of 8.2:15.8:10
Hybrid reaction is carried out in reactor, preparation solution hydrolyzes to obtain mixed phenylglycine, and the MIC reactor discharge port connects gas-liquid separation
Tank, the gas vent of knockout drum connect pressure gauge and show that system pressure, knockout drum are further connected with counterbalance valve to whole system
Carry out back pressure.
2. a kind of MIC reactor according to claim 1 prepares the new method of L-Phenylglycine precursor benzene glycolylurea, special
Sign is first to be pumped into the ammonium bicarbonate aqueous solution for accounting for its gross mass 60% when preparing, then flow set pumps three raw materials simultaneously
It is complete.
3. a kind of MIC reactor according to claim 1 prepares the new method of L-Phenylglycine precursor benzene glycolylurea, special
Respectively by ammonium bicarbonate aqueous solution, 30% Cymag, benzaldehyde respectively with 2800L/h, 940L/h, 600L/h when sign is to prepare
Flow be continuously pumped into MIC reactor.
4. a kind of MIC reactor according to claim 2 or 3 prepares the new method of L-Phenylglycine precursor benzene glycolylurea,
It is characterized in that the MIC inside reactor is inserted into 2205 stainless steel microchannel inserted sheet of nanoscale.
5. a kind of MIC reactor according to claim 4 prepares the new method of L-Phenylglycine precursor benzene glycolylurea, special
Sign is that the MIC inside reactor channel arranged in parallel, single channel size are constant.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910059874.7A CN109776424B (en) | 2019-01-22 | 2019-01-22 | Novel method for preparing L-phenylglycine precursor phenylhydantoin by using MIC reactor |
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| CN201910059874.7A CN109776424B (en) | 2019-01-22 | 2019-01-22 | Novel method for preparing L-phenylglycine precursor phenylhydantoin by using MIC reactor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111269134A (en) * | 2020-04-01 | 2020-06-12 | 九江中星医药化工有限公司 | Method for preparing phenylglycine and derivatives thereof |
| CN112250634A (en) * | 2020-10-22 | 2021-01-22 | 苏州亚科科技股份有限公司 | Preparation method of 4-phenylimidazole |
| CN114516811A (en) * | 2022-03-07 | 2022-05-20 | 浙江云涛生物技术股份有限公司 | Method for racemization reaction of phenylglycine in alkaline environment |
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| CN103086905A (en) * | 2011-09-07 | 2013-05-08 | 浙江云涛生物技术股份有限公司 | Preparation method for DL-phenylglycine |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111269134A (en) * | 2020-04-01 | 2020-06-12 | 九江中星医药化工有限公司 | Method for preparing phenylglycine and derivatives thereof |
| CN111269134B (en) * | 2020-04-01 | 2022-09-20 | 九江中星医药化工有限公司 | Preparation method of phenylglycine and derivatives thereof |
| CN112250634A (en) * | 2020-10-22 | 2021-01-22 | 苏州亚科科技股份有限公司 | Preparation method of 4-phenylimidazole |
| CN114516811A (en) * | 2022-03-07 | 2022-05-20 | 浙江云涛生物技术股份有限公司 | Method for racemization reaction of phenylglycine in alkaline environment |
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