CN208562196U - A kind of device producing concentrated formaldehyde - Google Patents

A kind of device producing concentrated formaldehyde Download PDF

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CN208562196U
CN208562196U CN201721234462.5U CN201721234462U CN208562196U CN 208562196 U CN208562196 U CN 208562196U CN 201721234462 U CN201721234462 U CN 201721234462U CN 208562196 U CN208562196 U CN 208562196U
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formaldehyde
tail gas
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steam
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王雪岭
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Jiangsu Dalton Petrochemical Technology Co Ltd
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Jiangsu Dalton Petrochemical Technology Co Ltd
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Abstract

The utility model relates to a kind of devices for producing concentrated formaldehyde, comprising: sequentially connected steam superheating unit, catalysis reaction member, steam generating unit and absorptive unit;Steam superheating unit upstream is connected with dimethoxym ethane vaporization unit and air pressurized unit.The utility model is by the rational design of apparatus structure, and the yield of the formaldehyde of 55~70wt% is up to 95% or more, and methanol and the total conversion ratio of dimethoxym ethane are up to 99.1% or more;The concentration for generating reaction selectivity up to 99.3% concentrated formaldehyde obtained as above of concentrated formaldehyde is 55% or more.Economic benefit is improved, investment is reduced, reduces the generation of waste water.The heat generated in technical process is subjected to self-sufficiency, energy consumption is reduced, simplifies technique, so that operation is easier.

Description

A kind of device producing concentrated formaldehyde
Technical field
The utility model relates to chemical production technical field more particularly to a kind of devices for producing concentrated formaldehyde.
Background technique
Paraformaldehyde is produced using formaldehyde as primary raw material, obtains solid formaldehyde by evaporation, concentration, through catalyzing and condensing, then Vacuum dried finished product.But during producing paraformaldehyde, formaldehyde has a large amount of dilute first by concentration and extraction Aldehyde generates, and how to handle dilute formaldehyde, has become the problem of paraformaldehyde manufacturer, handles dilute formaldehyde and provide in existing document In material, most published methods are only to convert environment permission for formaldehyde using chemical transformation from the angle of environmental protection The substance of discharge, or with the method for biochemical treatment, there are shortcomings for the dilute formaldehyde of these methods processing: conversion not exclusively, Due to the generation of side reaction, part formaldehyde is further converted to be existed in the form of formaldehyde and formates, therefore after conversion processing Solution can not direct emission;Formaldehyde is converted to formose class, is unable to recycling and reusing, results in waste of resources.Currently exist In formaldehyde downstream product production process, these dilute formalin some are concentrated again, and energy cost and investment are high, and what is had is dilute Formaldehyde, which is added in concentrated formaldehyde, is exchanged into the sale of commodity formaldehyde, but because market capacity is limited or the more demanding of market PARA FORMALDEHYDE PRILLS(91,95) can not It is fully utilized, the dilute formaldehyde having is further processed into methenamine or dimethoxym ethane (also known as formal or dimethoxy Methane), but because market is limited, economy is bad, causes this partial material to have no idea to be handled well, to make whole A downstream process is unsmooth.Dimethoxym ethane is originally used for gasoline addition, and market orientation instructs those skilled in the art to abandon to be contracted with first The less expensive formaldehyde of aldehyde production prices, after requirement must not add dimethoxym ethane in gasoline national standard, the city of dimethoxym ethane Field flow is dynamic to be deteriorated, sluggish market.
Formaldehyde multi-pass as reaction raw materials crosses the conventional method preparation of methanol oxidation, a large amount of due to being formed during reaction Water and keep the utilization rate of methanol low.Thus the maximum concentration of the formalin prepared is only 55wt%, to be obtained higher dense Degree is difficult.It is being that reaction raw materials prepare polyacetal resin, formaldehyde resin, phenolic resin, paraformaldehyde, urea with formaldehyde When closing object, it is desirable that the concentration of formaldehyde is as high as possible.In order to improve the concentration of formaldehyde, the prior art includes distillation or washs, or will Then formaldehyde reacts generation hemiacetal with alcohol must obtain formaldehyde enriched gas since concentration is not high enough by heating evaporation, this Cross the consersion unit of the quite stringent reaction condition of range request, it is also necessary to a large amount of energy consumption.
CN102329407A disclose it is a kind of produce paraformaldehyde be generate dilute formaldehyde circulation use technology, pass through object The means of reason break the change between the compound between methanol-formaldehyde in formaldehyde waste water, methanol-water and Formaldehyde-water-derivative Interaction and chemical balance relationship, realizes the separation of formaldehyde and water, but the oxidizable generation of formaldehyde in concentration process Formic acid concn, reduce formaldehyde yield not only influence after workshop section produce, also hide some dangers for production steady in a long-term, corrosion equipment is tight Weight, maintenance of equipment expend big.Therefore, find it is a kind of do not need special equipment can Efficient Cycle using dilute formaldehyde height it is pervasive The method of resource of property has great importance.
Utility model content
In view of problems of the prior art, one of the purpose of this utility model is to provide a kind of concentrated formaldehyde that produces Device, comprising: sequentially connected steam superheating unit, catalysis reaction member, steam generating unit and absorptive unit;The steam It crosses hot cell upstream and is connected with dimethoxym ethane vaporization unit and air pressurized unit.
Device described in the utility model includes: that fresh air enters air pressurized for producing the workflow of concentrated formaldehyde Unit enters dimethoxym ethane together with methanol and mixed steam with the dimethoxym ethane that dimethoxym ethane vaporization unit comes after being pressurizeed and crosses hot cell, Steam is further heated to overtemperature from saturation temperature by steam superheating unit, and it is single that obtained mixed steam enters catalysis reaction Member reacts: CH under the catalytic action of catalyst3OCH2OCH3+O2→3CH2O+H2O, the generated hot gas containing formaldehyde Further cool down in steam generating unit, waste heat for generating steam, the gaseous mixture after cooling enters the dense first of absorptive unit absorption Aldehyde is produced as product.
Preferably, the air pressurized unit includes pressurization blower.Air can be set in the upstream of pressurization blower Air blower first will enter back into pressurization blower after air pressure regulation, and stable air input is provided for described device.
Preferably, the steam superheating unit includes the feed opening for being set to middle part, for methanol to be added.
Preferably, the catalysis reaction member includes catalyst fixed bed, for generating formaldehyde and heating unit, is used for It heats described catalyst fixed bed.
Preferably, the catalyst includes iron-molybdic catalyst.
Preferably, the catalysis reaction member further includes heat-conducting medium, the heat generated for taking away catalysis reaction.
Preferably, the heat-conducting medium includes conduction oil and/or fuse salt.The heat that catalytic oxidation generates is by thermally conductive Medium is taken away.
Preferably, heat exchange unit is provided between the steam generating unit and steam superheating unit.Steam generating unit In cooling after gaseous mixture containing formaldehyde and steam superheating unit in dimethoxym ethane gas exchanged heat by heat exchanger after, drop Low energy consumption.
Preferably, the absorptive unit downstream connection has tail gas treating unit, and the tail gas treating unit includes and the external world The outlet of connection.
Preferably, the tail gas treating unit includes tail gas catalyzed processing unit.
Preferably, it is provided with shifting hot cell between the tail gas treating unit and the steam generating unit, is used for tail The heat of gas disposal unit is transferred to steam generating unit.
Preferably, the absorptive unit includes the circulating-heating unit for being set to the absorptive unit bottom, for absorbing Formaldehyde, the offgas outlet being set at the top of the absorptive unit for the output of tail gas, and are set in the middle part of the absorptive unit Reflux condensation mode unit, for further absorb formaldehyde.Reaction product gaseous mixture enters the circulating-heating list of absorptive unit bottom Member guarantees the formaldehyde liquid temperature absorbed up to 80 DEG C or more, and the concentration of absorption is 55~70wt%, and the formaldehyde of bottom is as product Extraction, unabsorbed formaldehyde gas further down cycles absorption, absorbing liquid in the reflux condensation mode unit in the middle part of absorptive unit It converges and in absorptive unit bottom, is equivalent to that formaldehyde gas formaldehyde gas after multistage absorption is substantially all to be absorbed.
Preferably, the absorptive unit includes absorption tower.
Preferably, circulation of tail gas unit is provided between the absorptive unit and the air pressurized unit.
Preferably, the offgas outlet of the absorptive unit respectively with the entrance of tail gas treating unit and the circulation of tail gas list The entrance connection of member.Contain oxygen in the tail gas that formaldehyde gas generates after absorbing formaldehyde, can directly pass through exhaust gas circulation system Returning air presser unit recycles in said device after being pressurizeed simultaneously with fresh air, can also enter at tail gas Reason unit further purifies, and including CO, dimethyl ether etc., other organic matters are all nontoxic by the oxygen oxidation transformation in tail gas Carbon dioxide and water, directly be vented, and simultaneous reactions release heat can supply steam generation facility generate steam when institute The heat needed.
In method using one of such as the utility model aim described device production formaldehyde, the dimethoxym ethane vaporization unit goes out Mouthful dimethoxym ethane steam flow be 80~200L/s, such as 80L/s, 90L/s, 100L/s, 110L/s, 120L/s, 130L/s, 140L/s, 150L/s, 160L/s, 170L/s, 180L/s, 190 or 200L/s etc..
Preferably, the air velocity of air pressurized unit outlet is 1000~2500L/s, such as 1000L/s, 1200L/s, 1400L/s, 1500L/s, 1800L/s, 2000L/s, 2200L/s, 2300L/s, 2400L/s or 2500L/s etc..
Preferably, it is described catalysis reaction member reaction temperature be 320~430 DEG C, such as 320 DEG C, 350 DEG C, 360 DEG C, 270 DEG C, 380 DEG C, 390 DEG C, 400 DEG C, 410 DEG C, 420 DEG C or 430 DEG C etc..
Preferably, the dimethoxym ethane steam and air are 0.2~0.28s/ times in the residence time of catalysis reaction member, example Such as 0.2s/ times, 0.21s/ times, 0.22s/ times, 0.23s/ times, 0.24s/ times, 0.25s/ times, 0.26s/ times, 0.27s/ times or 0.28s/ is inferior.
Preferably, the temperature of the circulating-heating unit is 100~150 DEG C, such as 100 DEG C, 105 DEG C, 110 DEG C, 115 DEG C, 120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C, 140 DEG C, 145 DEG C, 148 DEG C or 150 DEG C etc..
Preferably, the concentration of formaldehyde that the circulating-heating unit absorbs is 55~70wt%, such as 55wt%, 56wt%, 58wt%, 59wt%, 60wt%, 62wt%, 65wt%, 66wt%, 68wt%, 69wt% or 70wt% etc..
Preferably, it is preferably added to softened water at the top of the absorption plant, further absorbs formaldehyde gas.
As the preferred technical solution of the utility model, the device of the production concentrated formaldehyde includes: sequentially connected steam Cross hot cell, catalysis reaction member, steam generating unit and absorptive unit;Steam superheating unit upstream is connected with dimethoxym ethane Vaporization unit and air pressurized unit.The steam superheating unit includes the feed opening for being set to middle part, for methanol to be added;Institute State catalysis reaction member include it is catalyst fixed bed, for generating formaldehyde and heating unit, fixed for heating the catalyst Bed and heat-conducting medium, the heat generated for taking away catalysis reaction;Between the steam generating unit and steam superheating unit It is provided with heat exchange unit;The absorptive unit downstream connection has a tail gas treating unit, the tail gas catalyzed processing unit include with The outlet of extraneous connection is provided with shifting hot cell between the tail gas treating unit and the steam generating unit, be used for tail The heat of gas disposal unit is transferred to steam generating unit;The absorptive unit includes being set to following for the absorptive unit bottom Ring heating unit, for absorbing formaldehyde, the offgas outlet being set at the top of the absorptive unit for the output of tail gas, and is set The reflux condensation mode unit being placed in the middle part of the absorptive unit, for further absorbing formaldehyde;The absorptive unit and the air Be provided with circulation of tail gas unit between presser unit, the offgas outlet of the absorptive unit respectively with the entrance of tail gas treating unit It is connected with the entrance of the circulation of tail gas unit.
Compared with prior art, the utility model at least has the following beneficial effects:
1. the utility model is by the rational design of apparatus structure, the yield of the formaldehyde of 55~70wt% up to 95% or more, Methanol and the total conversion ratio of dimethoxym ethane are up to 99.1% or more;The reaction selectivity of concentrated formaldehyde is generated up to 99.3% dense first obtained as above The concentration of aldehyde is 55% or more.
2. the utility model realizes the preparation of high-concentration formaldehyde, the downstream product that PARA FORMALDEHYDE PRILLS(91,95) has high concentration to require, dense Compression process utility model device can reduce dilute formaldehyde that concentration generates, and consume energy as few as possible, it might even be possible to not throw Requirement can be directly reached by entering thermal energy.It increases economic efficiency, reduces investment, reduce the generation of waste water.
3. the heat generated in technical process is carried out self-supporting, drop by the connection relationship inside device by the utility model Low energy consumption, simplifies technique, so that operation is easier.
Detailed description of the invention
Fig. 1 is the schematic diagram of the device of the utility model embodiment production concentrated formaldehyde.
Signal: 1- pressurization blower is marked in figure;2- dimethoxym ethane vaporizer;3- superheater;4- catalyst reaction device;5- is changed Hot device;6- steam generator;The absorption tower 7-;8- circulation of tail gas device;The tail gas catalyzed processing system of 9-;10- moves hot device
The utility model is further described below.But following examples is only the simple example of the utility model Son, does not represent or limits the rights protection scope of the utility model, and the protection scope of the utility model is with claims It is quasi-.
Specific embodiment
Further illustrate the technical solution of the utility model below with reference to the accompanying drawings and specific embodiments.
For the utility model is better described, it is easy to understand the technical solution of the utility model, the typical case of the utility model But non-limiting embodiment is as follows, this is practical it will be clearly understood that the embodiment is only to aid in understanding by those skilled in the art It is novel, it is not construed as the concrete restriction to the utility model.
Embodiment 1
A kind of device producing concentrated formaldehyde, as shown in Figure 1, comprising: sequentially connected superheater 3, catalyst reaction device 4, Steam generator 6 and absorption tower 7.
Wherein, the upstream of superheater 3 is connected with dimethoxym ethane vaporizer 2 and pressurization blower 1;Superheater 3 includes being set to The feed opening at middle part, for methanol to be added;It include that fixed bed, heating device and heat-conducting medium are thermally conductive inside catalyst reaction device 4 Oil;Heat exchanger 5 is provided between superheater 3 and steam generator 6;The top on absorption tower 7 is connected with tail gas catalyzed processing system 9 With circulation of tail gas device 8, tail gas catalyzed processing system 9 is equipped with the outlet with extraneous connection;Tail gas catalyzed processing system 9 and steam It is provided between generator 6 and moves hot device 10;The bottom on absorption tower 7 is equipped with recirculation heater, and middle part is equipped with reflux condensate device.
Using the method for this device production formaldehyde, setting parameter is as follows:
Catalyst in fixed bed is iron-molybdic catalyst, and the dimethoxym ethane steam flow that dimethoxym ethane vaporizer 2 exports is 80L/ S, the air velocity that pressurization blower 1 exports are 1000L/s, and the reaction temperature of catalyst reaction device 4 is 330 DEG C, and dimethoxym ethane steams The residence time of vapour and air in catalyst reaction device 4 is 0.2s/ times;The temperature of 7 bottom of absorption tower is 100 DEG C.It absorbs The concentration of formaldehyde arrived is 55wt%.
Embodiment 2
Device is same as Example 1, and heat-conducting medium replaces with fuse salt, and design parameter is as follows:
Catalyst in fixed bed is iron-molybdic catalyst, and the dimethoxym ethane steam flow that dimethoxym ethane vaporizer 2 exports is 200L/ S, the air velocity that pressurization blower 1 exports are 2500L/s, and the reaction temperature of catalyst reaction device 4 is 380 DEG C, and dimethoxym ethane steams The residence time of vapour and air in catalyst reaction device 4 is 0.28s/ times;The temperature of 7 bottom of absorption tower is 150 DEG C.It absorbs The concentration of formaldehyde arrived is 56wt%.
Embodiment 3
Device is same as Example 1, and parameter is different, specific as follows:
The dimethoxym ethane steam flow that dimethoxym ethane vaporizer 2 exports is 100L/s, and the air velocity that pressurization blower 1 exports is 1500L/s, the reaction temperature of catalyst reaction device 4 are 380 DEG C, and dimethoxym ethane steam and air stop in catalyst reaction device 4 Staying the time is 0.22s/ times;The temperature of 7 bottom of absorption tower is 120 DEG C.Absorbing obtained concentration of formaldehyde is 64wt%.
Embodiment 4
Device is same as Example 1, and heat-conducting medium replaces with fuse salt, and design parameter is as follows:
The dimethoxym ethane steam flow that dimethoxym ethane vaporizer 2 exports is 180L/s, and the air velocity that pressurization blower 1 exports is 2100L/s, the reaction temperature of catalyst reaction device 4 are 380 DEG C, and dimethoxym ethane steam and air stop in catalyst reaction device 4 Staying the time is 0.26s/ times;The temperature of 7 bottom of absorption tower is 140 DEG C.Absorbing obtained concentration of formaldehyde is 65wt%.
Embodiment 5
Device is same as Example 1, and parameter is different, specific as follows:
The dimethoxym ethane steam flow that dimethoxym ethane vaporizer 2 exports is 150L/s, and the air velocity that pressurization blower 1 exports is 1700L/s, the reaction temperature of catalyst reaction device 4 are 400 DEG C, and dimethoxym ethane steam and air stop in catalyst reaction device 4 Staying the time is 0.24s/ times;The temperature of 7 bottom of absorption tower is 125 DEG C, and softened water is added in the top on absorption tower 7.What absorption obtained Concentration of formaldehyde is 70wt%.
Table 1 is the total conversion ratio of the methanol and dimethoxym ethane of each embodiment, reaction selectivity, the concentration of product concentrated formaldehyde.From Table 1 as can be seen that rational design of the utility model by apparatus structure, the yield of the formaldehyde of 55~70wt% up to 95% with On, methanol and the total conversion ratio of dimethoxym ethane are up to 99.1% or more;The reaction selectivity for generating concentrated formaldehyde is obtained as above up to 99.3% The concentration of concentrated formaldehyde is 55% or more.
Table 1
Conversion ratio Reaction selectivity Production concentration
Embodiment 1 99.1% 99.6% 55%
Embodiment 2 99.3% 99.6% 56%
Embodiment 3 99.3% 99.3% 64%
Embodiment 4 99.3% 99.4% 65%
Embodiment 5 99.3% 99.5% 70%
The Applicant declares that the utility model illustrates the detailed process equipment and work of the utility model through the foregoing embodiment Skill process, but the utility model is not limited to above-mentioned detailed process equipment and process flow, that is, does not mean that the utility model Above-mentioned detailed process equipment and process flow, which must be relied on, to be implemented.It should be clear to those skilled in the art, right Any improvement of the utility model, the addition of equivalence replacement and auxiliary element to each raw material of the utility model product, specific side The selection etc. of formula, all falls within the protection scope of the utility model and the open scope.

Claims (9)

1. a kind of device for producing concentrated formaldehyde characterized by comprising sequentially connected steam superheating unit, catalysis reaction are single Member, steam generating unit and absorptive unit;
Steam superheating unit upstream is connected with dimethoxym ethane vaporization unit and air pressurized unit;
The absorptive unit downstream connection has tail gas treating unit, and the tail gas treating unit includes the outlet with extraneous connection.
2. device as described in claim 1, which is characterized in that the air pressurized unit includes pressurization blower.
3. device as claimed in claim 1 or 2, which is characterized in that the steam superheating unit includes being set to adding for middle part Material mouth.
4. device as described in claim 1, which is characterized in that the catalysis reaction member includes catalyst fixed bed and heating Unit.
5. device as described in claim 1, which is characterized in that be arranged between the steam generating unit and steam superheating unit There is heat exchange unit.
6. device as described in claim 1, which is characterized in that the tail gas treating unit includes tail gas catalyzed processing unit;
Shifting hot cell is provided between the tail gas treating unit and the steam generating unit.
7. device as described in claim 1, which is characterized in that the absorptive unit includes being set to the absorptive unit bottom Circulating-heating unit, the offgas outlet being set at the top of the absorptive unit, and be set in the middle part of the absorptive unit return Flow condensing unit.
8. device as described in claim 1, which is characterized in that the absorptive unit includes absorption tower.
9. device as described in claim 1, which is characterized in that be arranged between the absorptive unit and the air pressurized unit There is circulation of tail gas unit;
The offgas outlet of the absorptive unit connects with the entrance of the entrance of tail gas treating unit and the circulation of tail gas unit respectively It connects.
CN201721234462.5U 2017-09-25 2017-09-25 A kind of device producing concentrated formaldehyde Active CN208562196U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113061219A (en) * 2021-03-29 2021-07-02 无锡熙源工程技术有限公司 Paraformaldehyde production process

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113061219A (en) * 2021-03-29 2021-07-02 无锡熙源工程技术有限公司 Paraformaldehyde production process

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