CN203448102U - Gas-liquid spraying circulating reaction device for preparing glyoxylic acid by oxygen oxidization method - Google Patents
Gas-liquid spraying circulating reaction device for preparing glyoxylic acid by oxygen oxidization method Download PDFInfo
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- CN203448102U CN203448102U CN201320532444.0U CN201320532444U CN203448102U CN 203448102 U CN203448102 U CN 203448102U CN 201320532444 U CN201320532444 U CN 201320532444U CN 203448102 U CN203448102 U CN 203448102U
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Abstract
The utility model discloses a gas-liquid spraying circulating reaction device for preparing glyoxylic acid by an oxygen oxidization method, which solves the problems that a lot of NOX tail gas is generated in the production process, the environment is polluted, the consumption amount of nitric acid is great and the like in the prior art. The gas-liquid spraying circulating reaction device is characterized in that a gas-liquid mixing and spraying circulating device, a liquid seal alarming device and an oxygen supplying device are additionally arranged on a reaction kettle (7) on the basis of traditional production equipment composed of the reaction kettle (7), an agitating paddle (10), a heating steam valve (5), a cooling water valve (6), a feeding opening (3), a discharging valve (8) and the like. According to the gas-liquid spraying circulating reaction device, the oxygen oxidization method is carried out in a normal-pressure reaction kettle and the security coefficient is increased; the consumption amount of nitric acid is reduced greatly and the exhausting amount of NOX tail gas is also greatly reduced; the yield of glyoxylic acid is improved greatly.
Description
One, technical field
The utility model belongs to medication chemistry production equipment, relates in particular to a kind of dioxygen oxidation legal system for the gas-liquid injection circular response device of glyoxalic acid.
Two, background technology
Glyoxalic acid (OHC-COOH), is a kind of broad-spectrum chemical products, is mainly used in the products such as synthetic 4-Hydroxyphenyl hydantoin, vanillic aldehyde and hydroxyl phosphine carboxylic acid.Along with the development in glyoxalic acid downstream product market, it has become large chemical products that production scale reaches tens thousand of tons, and market demand steady-state growth.
Have the method for industrial prospect mainly based on different oxidants such as adopting nitric acid, nitrogen oxide, oxygen, chlorine and combination thereof, to be oxidized glyoxal in inorganic acid medium, production technology has also experienced many generations and has improved.The improved nitric acid oxidation method of current industrial extensive use, also deposits and produces in process of production a large amount of NO
xtail gas, the problem such as contaminated environment and nitric acid consumption are large.For how effectively reducing NO
xtail gas pollution and nitric acid consumption, in the existing way of chemosynthesis technical field as patent of invention < < technology for absorbing tail gas of glyoxalic acid production > >, 200810049919.4, Xie Jianzhong.Adopt three grades of absorption plants to absorb, front I and II is absorbing pure water, and the third level is that 10-20% sodium hydroxide solution absorbs.But the method also exists nitric acid consumption large, the problem such as the large and absorption equipment of vent gas treatment amount is huge; The synthetic method > > of patent of invention < < preparing glyoxalic acid solution by oxygen catalytic oxidation of glyoxal with nitrogen oxide and for example, 200410096499.7, Zhou Zhiming.It is in closed reactor, uses nitrogen oxide catalysis, uses dioxygen oxidation glyoxal water solution to prepare glyoxalic acid solution.But the method is to carry out in closed container, can gather because of raw material, react and set off an explosion suddenly, there is very large potential safety hazard.With the comparison of traditional nitric acid oxidation glyoxal method, its equipment requirement is higher, and equipment cost increases, and operation easier increases.This patent is still unrealized industrialization so far.
Three, summary of the invention
The purpose of this utility model is exactly in order to provide a kind of in original normal-pressure reaction kettle, by the method for nitrogen oxide oxygen catalytic oxidation glyoxal preparation glyoxalic acid, realizes industrialized dioxygen oxidation legal system for the gas-liquid injection circular response device of glyoxalic acid.
The technical solution of the utility model is: it is on the conventional production equipment basis consisting of reactor, paddle, heating steam valve, cooling water valve, charging aperture and outlet valve, has set up gas-liquid mixed ejector cycle device, fluid-tight warning device and oxygen feedway on reactor.Described gas-liquid mixed ejector cycle device is comprised of air pump, frequency converter, gas-liquid mixing ejector and pipeline, the inlet pipeline of air pump is connected with the breather pipe on reactor kettle cover, its port of export is connected with the gas inlet tube of gas-liquid mixing ejector, the liquid inlet tube of gas-liquid mixing ejector is connected or directly inserts reactor inner bottom part with reactor bottom discharge nozzle, and gas-liquid mixture fluid outlet is communicated with the inlet tube on reactor kettle cover; Described fluid-tight warning device is to be connected with the liquid seal trough that alarm is housed by pipeline by being arranged on still upper part of the cover blast pipe; Described oxygen feedway is comprised of with the pipeline with oxygen valve being connected with reactor top the weigher that is arranged on the placement oxygen bottle of reactor one side; Heating steam valve and boiler steam pipeline on reactor join, and cooling water valve is connected with cooling water pipeline, and the entrance point of oxygen valve is connected with the oxygen bottle being placed on weigher, and reactor bottom sets out material valve.Paddle top in reactor is provided with Gas Stirring blade.
The beneficial effects of the utility model are: realized dioxygen oxidation method and carried out in normal-pressure reaction kettle, saved equipment investment, reduced operation easier, increased safety coefficient; Compare with traditional nitric acid oxidation method, both greatly reduced the consumption of nitric acid, also greatly reduced NO
xexhaust emissions amount, has also improved the yield of product glyoxalic acid.
Below in conjunction with accompanying drawing, the utility model is described in further detail.
Four, accompanying drawing explanation:
Fig. 1 is structural representation of the present utility model.
In figure: 1 is frequency converter, 2 is air pump, and 3 is charging aperture, 4 is blast pipe, and 5 is heating steam valve, and 6 is cooling water valve, 7 is reactor, and 8 is outlet valve, and 9 is weigher, 10 is liquid agitation blade, 11 is Gas Stirring blade, and 12 is gas-liquid mixing ejector, and 13 is oxygen valve, 14 is alarm, and 15 is liquid seal trough.
Five, the specific embodiment
As shown in Figure 1, on the conventional production equipment basis being formed by reactor, paddle, heating steam valve, cooling water valve, charging aperture and outlet valve, gas-liquid mixed ejector cycle device, fluid-tight warning device and oxygen feedway on reactor 7, have been set up.Described gas-liquid mixed ejector cycle device is comprised of air pump 2, frequency converter 1, gas-liquid mixing ejector 12 and pipeline, the inlet pipeline of air pump 2 is connected with the breather pipe on reactor 7 kettle covers, its port of export is connected with the gas inlet tube of gas-liquid mixing ejector 12, the liquid inlet tube of gas-liquid mixing ejector 12 is connected or directly inserts reactor 7 inner bottom parts with reactor bottom discharge nozzle, and gas-liquid mixture fluid outlet is communicated with the inlet tube on reactor kettle cover; Described fluid-tight warning device is to be connected with the liquid seal trough 15 that alarm 14 is housed by pipeline by being arranged on still upper part of the cover blast pipe (4); Described oxygen feedway is comprised of with the pipeline with oxygen valve 13 being connected with reactor top the weigher 9 that is arranged on the placement oxygen bottle of reactor 7 one sides; Heating steam valve 5 on reactor 7 joins with boiler steam pipeline, and cooling water valve 6 is connected with cooling water pipeline, and the entrance point of oxygen valve 13 is connected with the oxygen bottle being placed on weigher, and outlet valve 8 is established in reactor 7 bottoms.Paddle top in reactor 7 is provided with Gas Stirring blade 11.While implementing the utility model, a certain amount of 20-40% glyoxal solution is added in reactor 7, appropriate technical hydrochloric acid and water are dropped into reactor 7, under stirring, crack heating steam valve 5, while being slowly warming up to 55 ℃, cuts out heating steam valve 5.Open oxygen valve 13 and pass into oxygen, drive away after reactor 7 top air, close oxygen valve 13.Drip rare nitric acid that appropriate water absorbs tail gas gained, reaction starts immediately, there is rufous NO gas to emit, drip rare nitric acid complete, drip immediately 40% nitric acid preparing in advance, when temperature rises to 60 ℃, open cooling water valve 6, stop dripping 40% nitric acid, open again oxygen valve 13, booster air pump 2, maintain reaction temperature at 55-65 ℃, reaction pressure is normal pressure, when system normal pressure alarm equipment alarm or temperature are over 61 ℃, increase cooling water flow or reduce oxygen flow, when system negative pressure alarm equipment alarm or temperature drop to below 59 ℃, reduce cooling water flow, increase oxygen flow or drip nitric acid and supplement nitrogen oxide, when dripping oxygen sum that oxygen that nitric acid emits in oxidation reaction process and steel cylinder pass into and reach chemical reaction equivalent point, stop logical oxygen, insulation reaction 1 hour, be cooled to 0-5 ℃, separate out white crystal, filter to obtain oxalic acid, filtrate is glyoxylic acid solution.
Claims (3)
1. a dioxygen oxidation legal system is for the gas-liquid injection circular response device of glyoxalic acid, it comprises reactor (7), paddle (10), heating steam valve (5), cooling water valve (6), charging aperture (3) and outlet valve (8), it is characterized in that: on reactor (7), be provided with gas-liquid mixed ejector cycle device, fluid-tight warning device and oxygen feedway.
2. dioxygen oxidation legal system according to claim 1 is for the gas-liquid injection circular response device of glyoxalic acid, it is characterized in that: described gas-liquid mixed ejector cycle device is by air pump (2), frequency converter (1), gas-liquid mixing ejector (12) and pipeline form, the inlet pipeline of air pump (2) is connected with the breather pipe on reactor (7) kettle cover, its port of export is connected with the gas inlet tube of gas-liquid mixing ejector (12), the liquid inlet tube of gas-liquid mixing ejector (12) is connected or directly inserts reactor (7) inner bottom part with reactor bottom discharge nozzle, gas-liquid mixture fluid outlet is communicated with the inlet tube on reactor kettle cover, described fluid-tight warning device is to be connected with the liquid seal trough (15) that alarm (14) are housed by pipeline by being arranged on still upper part of the cover blast pipe (4), described oxygen feedway is comprised of with the pipeline of the band oxygen valve (13) being connected with reactor top the weigher (9) that is arranged on the placement oxygen bottle of reactor (7) one sides, heating steam valve (5) on reactor (7) joins with boiler steam pipeline, and cooling water valve (6) is connected with cooling water pipeline, and the entrance point of oxygen valve (13) is connected with the oxygen bottle being placed on weigher, and outlet valve (8) is established in reactor (7) bottom.
3. dioxygen oxidation legal system according to claim 2, for the gas-liquid injection circular response device of glyoxalic acid, is characterized in that: the paddle top in reactor (7) is provided with Gas Stirring blade (11).
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106179150A (en) * | 2016-07-23 | 2016-12-07 | 河南新天地药业股份有限公司 | A kind of association response device of Biformyl oxidation synthesis glyoxylate |
CN108609618A (en) * | 2014-12-04 | 2018-10-02 | 夏雨 | Diamond retracting device |
CN111068476A (en) * | 2019-12-14 | 2020-04-28 | 汪子夏 | NO in process of dissolving metal by nitric acidXTail gas treatment device and method and terminal |
-
2013
- 2013-08-29 CN CN201320532444.0U patent/CN203448102U/en not_active Expired - Fee Related
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108609618A (en) * | 2014-12-04 | 2018-10-02 | 夏雨 | Diamond retracting device |
CN108609618B (en) * | 2014-12-04 | 2019-09-13 | 泉州台商投资区五季网络有限公司 | Diamond recyclable device |
CN106179150A (en) * | 2016-07-23 | 2016-12-07 | 河南新天地药业股份有限公司 | A kind of association response device of Biformyl oxidation synthesis glyoxylate |
CN111068476A (en) * | 2019-12-14 | 2020-04-28 | 汪子夏 | NO in process of dissolving metal by nitric acidXTail gas treatment device and method and terminal |
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Granted publication date: 20140226 Termination date: 20140829 |
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