CN104610031A - Production method of high-concentration formaldehyde - Google Patents
Production method of high-concentration formaldehyde Download PDFInfo
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- CN104610031A CN104610031A CN201410852864.6A CN201410852864A CN104610031A CN 104610031 A CN104610031 A CN 104610031A CN 201410852864 A CN201410852864 A CN 201410852864A CN 104610031 A CN104610031 A CN 104610031A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/37—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
- C07C45/38—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups being a primary hydroxyl group
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/80—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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Abstract
The invention provides a production method of high-concentration formaldehyde. The production method of the high-concentration formaldehyde comprises the following steps: methanol, air and water vapor are mixed and purified and then tangently enter an oxygenizer end socket, wherein a V-shaped distributor is arranged inside the oxygenizer end socket; after mixed gas is separated from condensate inside the V-shaped distributor, the mixed gas enters the oxygenize; under conditions of 10-20kap and 610-650 DEG C, the mixed gas is in contact with a silver catalyst, oxidation and dehydrogenation reaction is performed on methanol to generate formaldehyde gas; after the formaldehyde gas is absorbed, unabsorbed tail gas is separated from liquid by a gas-liquid separator, is sent into a tail gas processor and is burned; generated flue gas is pressurized by a blower, is mixed with methanol, air and water vapor and is then reoxygenized. The production method is simple; due to the adoption of the production method, high-concentration and high-quality formaldehyde can be produced and energy consumption can be reduced; the production method is high in practicality.
Description
Technical field
The present invention relates to prepn. of formaldehyde field, specifically a kind of production method of high-concentration formaldehyde.
Background technology
At present, generally all use methyl alcohol to carry out oxidation as raw material with the domestic production to industrial formol abroad to obtain.Utilize methyl alcohol to carry out air oxidation process production formaldehyde and mainly contain two kinds of diverse ways: the first adopts silver catalyst " methyl alcohol overflow method ", also claims " silver-colored catalysis method " (being called for short " silver-colored method "); The second adopts iron-molybdenum oxide catalyzer " air excess method ", also claims " iron molybdenum catalysis method " (being called for short " iron molybdenum method ").Adopt iron molybdenum method to produce the general throughput of device of formaldehyde comparatively large, methanol conversion can reach 95%-99%, and methanol consumption is low, and does not need water distilling apparatus, can produce high-concentration formaldehyde, low, the catalyzer long service life of alcohol content in formaldehyde finished product.But shortcoming is that one-time investment is large, power consumption is high, and cost is large.The technique that silver method produces formaldehyde is simple, and less investment, regulating power are strong, formic acid content is few in product, but shortcoming is that methanol conversion is low, unit consumption is high, catalyst life is short, requires high to methanol purity, and in formaldehyde finished product, methanol content is high.
China's silver method is produced formaldehyde course decades and can be divided 2 stages.
First stage, in the 50-60 age in 20th century, adopt float stone silver catalyst, obtain formalin by methanol oxidation Oxidative Dehydrogenation, this method energy consumption is large, and material consumption is high, and average material consumption is at 540kg/t.
Subordinate phase, so far, the silver-colored method based on catalyst for electrolytic silver produces formaldehyde technology to 20 century 70s.Formaldehyde industry of this one-phase China, under colleague makes joint efforts, is all greatly improved and develops in production capacity, production technology or equipment, energy-conservation and automatic control etc.Due to improving technique and equipment, adopt novel material, new technology, make formaldehyde production device become " not consuming vapour type " and " supplying steam type outward " by original " consumption vapour type ", energy consumption significantly reduces.Material consumption is also down to existing 455kg/t by former 540kg/t, but compares still with iron processes that there is a big difference.Lower consumption again if on catalyst preparing, chemical technique and key equipment, reform is not very difficult, production high density, high-quality formaldehyde.
Summary of the invention
The object of the invention is the production method providing a kind of high-concentration formaldehyde according to the deficiencies in the prior art, can produce the formaldehyde of high density, high-quality by the method, and energy consumption is low, cost is low.
The present invention is achieved through the following technical solutions: a kind of production method of high-concentration formaldehyde, and its step comprises:
Methyl alcohol, air, water vapor mixing tangent line after purification are entered oxidizer end socket, the built-in V-type sparger of oxidizer end socket, mixed gas is in V-type sparger after separating and condensing liquid, mixed gas enters oxidizer again, contact with silver catalyst under 10-20kpa with 610 DEG C of-650 DEG C of conditions, oxidation occurs methyl alcohol and dehydrogenation reaction generates formaldehyde gas; Above-mentioned formaldehyde gas first enters first grade absorption tower at the bottom of tower, formalin is discharged by first order absorption tower bottom with after the reverse absorption formaldehyde of absorption liquid, absorption liquid again through two-level absorption tower, is added by two-level absorption tower top and carries out reverse absorption by formaldehyde gas after the discharge of first order absorption tower top; The unabsorbed tail gas in two-level absorption tower top goes out to send in exhaust gas treating device after liquid through gas-liquid separator separates and burns, and delivers to mix with methyl alcohol, air, water vapor to be oxidized after the flue gas of generation is pressurizeed by gas blower again.
Preferably, the rare formalin pump at the bottom of two-level absorption tower is got rear section and is looped back two-level absorption tower tower top absorption formaldehyde gas, and another part sends into the absorption liquid that first grade absorption tower makes first grade absorption tower.
Preferably, the flue gas produced that burns in described exhaust gas treating device first wash through water wash column and is cooled to 0-100 DEG C, then is delivered to by gas blower pressurization after tail gas buffer, cyclonic separator removing water coolant and mix with methyl alcohol, air, water vapor.
Preferably, after described flue gas mixes with methyl alcohol, air, water vapor, progressively adjust batching quantity of steam according to oxidizing temperature.
Tool of the present invention has the following advantages and positively effect: (1) the built-in V-type sparger of oxidizer end socket can remove the water of condensation in mixed gas, and make gas distribution evenly, catalyzer silver powder can not dispel by mixed gas, and oxidation, dehydrogenation reaction are more abundant, and oxidizing temperature is more stable.(2) first grade absorption tower replenisher delivers to first grade absorption tower top, contacts, make absorption more abundant by sparger and formaldehyde gas are reverse.(3) remaining containing trace formaldehyde, methyl alcohol, CO, CO after absorbing
2, CH
4with a large amount of N
2, H
2deng tail gas send into exhaust gas treating device hearth combustion.Make that system is safer, environmental protection, energy-conservation.(4) adopt the flue gas after water wash column washing cleaner, the work-ing life of catalysis silver can be ensured.(5) flue gas pipeline arranges gas-liquid separator, surge tank makes flue gas water content foreign material reduce, and flue gas pressures is more stable.(6) flue gas adds system, and flue gas can replace water vapor to play thermal barrier, reduces side reaction, formaldehyde content can be made to reach more than 52%.(7) flue gas can reduce the aerial explosive range of methyl alcohol, favourable safety in production.(8) flue gas can suppress side reaction, reduces oxygen temperature thus reduces energy consumption.
The inventive method is simple, can produce the formaldehyde of high density high-quality, and can reduce energy consumption, have very strong practicality.
Embodiment
By the following specific examples further illustrate the invention:
Embodiment 1
Methyl alcohol, air, water vapor mixing tangent line after purification are entered oxidizer end socket, the built-in V-type sparger of oxidizer end socket, mixed gas is in V-type sparger after separating and condensing liquid, mixed gas enters oxidizer again, contact with silver catalyst under 10kpa with 610 DEG C of DEG C of conditions, oxidation occurs methyl alcohol and dehydrogenation reaction generates formaldehyde gas.Formaldehyde gas first enters first grade absorption tower at the bottom of tower, formalin is discharged by first order absorption tower bottom with after the reverse absorption formaldehyde of absorption liquid, formaldehyde gas from first order absorption tower top discharge after again through two-level absorption tower, absorption liquid is added by two-level absorption tower top and carries out reverse absorption, rare formalin pump at the bottom of two-level absorption tower is got rear section and is looped back two-level absorption tower tower top absorption formaldehyde gas, and another part sends into the absorption liquid that first grade absorption tower makes first grade absorption tower; The unabsorbed tail gas in two-level absorption tower top goes out to send in exhaust gas treating device after liquid through gas-liquid separator separates and burns, the flue gas produced is first after water wash column washs and is cooled to 0-30 DEG C, flue gas enters surge tank and cyclonic separator separating and condensing water and foreign material, pressurizeed to deliver to by gas blower and mix with methyl alcohol, air, water vapor, by the proportioning according to temperature adjustment air and steam after flue gas imports.
Embodiment 2
Methyl alcohol, air, water vapor mixing tangent line after purification are entered oxidizer end socket, the built-in V-type sparger of oxidizer end socket, mixed gas is in V-type sparger after separating and condensing liquid, mixed gas enters oxidizer again, contact with silver catalyst under 15kpa with 650 DEG C of conditions, oxidation occurs methyl alcohol and dehydrogenation reaction generates formaldehyde gas.Formaldehyde gas first enters first grade absorption tower at the bottom of tower, formalin is discharged by first order absorption tower bottom with after the reverse absorption formaldehyde of absorption liquid, formaldehyde gas from first order absorption tower top discharge after again through two-level absorption tower, absorption liquid is added by two-level absorption tower top and carries out reverse absorption, rare formalin pump at the bottom of two-level absorption tower is got rear section and is looped back two-level absorption tower tower top absorption formaldehyde gas, and another part sends into the absorption liquid that first grade absorption tower makes first grade absorption tower; The unabsorbed tail gas in two-level absorption tower top goes out to send in exhaust gas treating device after liquid through gas-liquid separator separates and burns, the flue gas produced is first after water wash column washs and is cooled to 20-80 DEG C, flue gas enters surge tank and cyclonic separator separating and condensing water and foreign material, pressurizeed to deliver to by gas blower and mix with methyl alcohol, air, water vapor, by the proportioning according to temperature adjustment air and steam after flue gas imports.
Embodiment 3
Methyl alcohol, air, water vapor mixing tangent line after purification are entered oxidizer end socket, the built-in V-type sparger of oxidizer end socket, mixed gas is in V-type sparger after separating and condensing liquid, mixed gas enters oxidizer again, contact with silver catalyst under 20kpa with 630 DEG C of conditions, oxidation occurs methyl alcohol and dehydrogenation reaction generates formaldehyde gas.Formaldehyde gas first enters first grade absorption tower at the bottom of tower, formalin is discharged by first order absorption tower bottom with after the reverse absorption formaldehyde of absorption liquid, formaldehyde gas from first order absorption tower top discharge after again through two-level absorption tower, absorption liquid is added by two-level absorption tower top and carries out reverse absorption, rare formalin pump at the bottom of two-level absorption tower is got rear section and is looped back two-level absorption tower tower top absorption formaldehyde gas, and another part sends into the absorption liquid that first grade absorption tower makes first grade absorption tower; The unabsorbed tail gas in two-level absorption tower top goes out to send in exhaust gas treating device after liquid through gas-liquid separator separates and burns, the flue gas produced is first after water wash column washs and is cooled to 60-100 DEG C, flue gas enters surge tank and cyclonic separator separating and condensing water and foreign material, pressurizeed to deliver to by gas blower and mix with methyl alcohol, air, water vapor, by the proportioning according to temperature adjustment air and steam after flue gas imports.
Embodiment 4
Traditional technology: methyl alcohol, air, water vapor mixing tangent line after purification are entered oxidizer end socket, the built-in V-type sparger of oxidizer end socket, mixed gas is in V-type sparger after separating and condensing liquid, mixed gas enters oxidizer again, contact with silver catalyst under 15kpa with 650 DEG C of conditions, oxidation occurs methyl alcohol and dehydrogenation reaction generates formaldehyde gas.The formaldehyde gas of generation is sent into inhale in tower and carries out absorption operation.Unabsorbed gases sends into the burning of tail stove, flue gas emptying.
Embodiment 5
Tail gas absorption technology: methyl alcohol, air, water vapor mixing tangent line after purification are entered oxidizer end socket, the built-in V-type sparger of oxidizer end socket, mixed gas is in V-type sparger after separating and condensing liquid, mixed gas enters oxidizer again, contact with silver catalyst under 15kpa with 650 DEG C of conditions, oxidation occurs methyl alcohol and dehydrogenation reaction generates formaldehyde gas.The formaldehyde gas of generation is sent into inhale in tower and carries out absorption operation.Unabsorbed gases is delivered to mix with methyl alcohol, air, water vapor via gas blower pressurization and is sent into oxidizer.
By the traditional technology of the technique of embodiments of the invention 1-3 and embodiment 4, the tail gas absorption technology contrast of embodiment 5, result is as shown in table 1:
Table 1 present invention process and traditional technology, tail gas absorption technology contrast
As can be seen from Table 1, method of the present invention can produce high density, high-quality methyl alcohol, and material consumption, energy consumption are low, and throughput is high.
For those skilled in the art, under the prerequisite not departing from embodiment of the present invention principle, can also make some improvements and modifications, these improvements and modifications are also considered as the protection domain of the embodiment of the present invention.
Claims (4)
1. a production method for high-concentration formaldehyde, its step comprises:
Methyl alcohol, air, water vapor mixing tangent line after purification are entered oxidizer end socket, the built-in V-type sparger of oxidizer end socket, mixed gas is in V-type sparger after separating and condensing liquid, mixed gas enters oxidizer again, contact with silver catalyst under 10-20kpa with 610 DEG C of-650 DEG C of conditions, oxidation occurs methyl alcohol and dehydrogenation reaction generates formaldehyde gas; Above-mentioned formaldehyde gas first enters first grade absorption tower at the bottom of tower, formalin is discharged by first order absorption tower bottom with after the reverse absorption formaldehyde of absorption liquid, absorption liquid again through two-level absorption tower, is added by two-level absorption tower top and carries out reverse absorption by formaldehyde gas after the discharge of first order absorption tower top; The unabsorbed tail gas in two-level absorption tower top goes out to send in exhaust gas treating device after liquid through gas-liquid separator separates and burns, and delivers to mix with methyl alcohol, air, water vapor to be oxidized after the flue gas of generation is pressurizeed by gas blower again.
2. the production method of high-concentration formaldehyde according to claim 1, it is characterized in that: the rare formalin pump at the bottom of two-level absorption tower is got rear section and looped back two-level absorption tower tower top absorption formaldehyde gas, and another part sends into the absorption liquid that first grade absorption tower makes first grade absorption tower.
3. the production method of high-concentration formaldehyde according to claim 1, it is characterized in that: the flue gas produced that burns in described exhaust gas treating device first wash through water wash column and is cooled to 0-100 DEG C, then delivered to by gas blower pressurization after tail gas buffer, cyclonic separator removing water coolant and mix with methyl alcohol, air, water vapor.
4. the production method of high-concentration formaldehyde according to claim 1, is characterized in that: after described flue gas mixes with methyl alcohol, air, water vapor, progressively adjusts batching quantity of steam according to oxidizing temperature.
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Cited By (7)
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CN106268247A (en) * | 2015-05-22 | 2017-01-04 | 中国科学院大连化学物理研究所 | A kind of catalytic absorption method of formaldehyde |
CN107200682A (en) * | 2017-07-12 | 2017-09-26 | 广东奕宏化工有限公司 | A kind of improved Formaldehyde Production system |
CN107501060A (en) * | 2017-08-24 | 2017-12-22 | 开封龙宇化工有限公司 | A kind of concentrated formaldehyde production technology |
CN107827720A (en) * | 2017-10-24 | 2018-03-23 | 安徽省福泰精细化工有限责任公司 | A kind of production method for improving concentration of formaldehyde |
CN111253229A (en) * | 2020-03-31 | 2020-06-09 | 山东明化新材料有限公司 | Formaldehyde pyridine hydrogen peroxide coproduction method |
CN112479845A (en) * | 2020-11-09 | 2021-03-12 | 潍坊惠丰化工有限公司 | High-concentration formaldehyde production device and production process |
CN114621072A (en) * | 2022-03-09 | 2022-06-14 | 赛鼎工程有限公司 | Process for producing concentrated formaldehyde by oxidizing methylal and methanol |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106268247A (en) * | 2015-05-22 | 2017-01-04 | 中国科学院大连化学物理研究所 | A kind of catalytic absorption method of formaldehyde |
CN107200682A (en) * | 2017-07-12 | 2017-09-26 | 广东奕宏化工有限公司 | A kind of improved Formaldehyde Production system |
CN107501060A (en) * | 2017-08-24 | 2017-12-22 | 开封龙宇化工有限公司 | A kind of concentrated formaldehyde production technology |
CN107827720A (en) * | 2017-10-24 | 2018-03-23 | 安徽省福泰精细化工有限责任公司 | A kind of production method for improving concentration of formaldehyde |
CN107827720B (en) * | 2017-10-24 | 2021-02-26 | 安徽省福泰精细化工有限责任公司 | Production method for improving concentration of formaldehyde |
CN111253229A (en) * | 2020-03-31 | 2020-06-09 | 山东明化新材料有限公司 | Formaldehyde pyridine hydrogen peroxide coproduction method |
CN111253229B (en) * | 2020-03-31 | 2022-08-30 | 山东明化新材料有限公司 | Formaldehyde pyridine hydrogen peroxide coproduction method |
CN112479845A (en) * | 2020-11-09 | 2021-03-12 | 潍坊惠丰化工有限公司 | High-concentration formaldehyde production device and production process |
CN114621072A (en) * | 2022-03-09 | 2022-06-14 | 赛鼎工程有限公司 | Process for producing concentrated formaldehyde by oxidizing methylal and methanol |
CN114621072B (en) * | 2022-03-09 | 2023-12-01 | 赛鼎工程有限公司 | Process method for producing concentrated formaldehyde by oxidizing methylal and methanol |
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Address after: 432401 No. 93 East Beijing Road, Shacheng District, Ezhou City, Hubei Province Patentee after: Andomai Co., Ltd. Address before: 432401 No. 93 East Beijing Road, Shacheng District, Ezhou City, Hubei Province Patentee before: Hubei Shalongda Co., Ltd. |