CN109574820B - Production method of formaldehyde - Google Patents
Production method of formaldehyde Download PDFInfo
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- CN109574820B CN109574820B CN201811504619.0A CN201811504619A CN109574820B CN 109574820 B CN109574820 B CN 109574820B CN 201811504619 A CN201811504619 A CN 201811504619A CN 109574820 B CN109574820 B CN 109574820B
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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
Abstract
The invention relates to a production method of formaldehyde, which comprises the following steps: 1) the reactor is composed of a pre-reactor, a first reactor and a second reactor which are connected in series, and the mixed gas sequentially passes through the pre-reactor, the first reactor and the second reactor; 2) the pre-reactor temperature is 140-150 ℃, the first reactor temperature is 150-270 ℃, and the second reactor temperature is 275-425 ℃. The absorption tower is formed by connecting a first absorption tower, a second absorption tower and a third absorption tower in series; the absorption liquid of the first absorption tower circulates to extract finished formaldehyde, the absorption liquid of the second absorption tower circulates to extract the circulating liquid to the first absorption tower for absorption, the absorption liquid of the third absorption tower adopts desalted water for absorption, and the absorption liquid circulates to extract the circulating liquid to the second absorption tower for absorption. The invention has the following advantages: 1. can directly produce formaldehyde with 55 percent of content, the acid detection is less than or equal to 0.005 percent, and the methanol content is less than or equal to 0.5 percent; 2. all iron molybdenum catalysts can be used; 3. the high-efficiency and low-consumption operation of the system is promoted, the production benefit is improved, and the production cost is reduced.
Description
Technical Field
The invention belongs to the technical field of chemical production, and relates to a production method of formaldehyde.
Background
Formaldehyde, chemical formula HCHO, formula weight 30.03, also known as formaldehyde. Colorless gas, special pungent odor, and irritation to human eye and nose, with relative gas density of 1.067 and air = 1) and liquid density of 0.815g/cm under thin-20 deg.C. Melting point-92 deg.C, boiling point-19.5 deg.C. Is easily soluble in water and ethanol. Aqueous solutions, up to 55% strength, usually 40%, are known as formalin (formalin) which is a colorless liquid with a pungent odor. The formaldehyde can be obtained by dehydrogenation or oxidation of methanol under the catalysis of metals such as silver, copper and the like, and can also be separated from hydrocarbon oxidation products. It is used as raw material for preparing agricultural chemicals and disinfectant, such as phenolic resin, urea-formaldehyde resin, vinylon, urotropine, pentaerythritol and dye. Formaldehyde is an important basic organic chemical raw material, has become a chemical product for large-scale production and consumption, and is widely used in chemical industry, medicine, textile, wood processing and petroleum industry. Modern industrial formaldehyde production mainly adopts an oxidation preparation process taking methanol as a raw material, and since the iron-molybdenum oxide catalyst is used for industrial production of formaldehyde by methanol oxidation in 1952, the iron-molybdenum oxide catalyst is widely developed and utilized due to the advantages of the performance of the iron-molybdenum oxide catalyst.
At present, the iron-molybdenum catalyst is imported mainly from sources, the supply price of foreign catalysts is high, and along with the gradual increase of market demand, the contradiction is more prominent, so that the research and development of the iron-molybdenum oxide catalyst capable of using all iron-molybdenum oxides are very important.
The invention content is as follows:
the invention aims to overcome the problems in the prior art and provides a formaldehyde production method. The invention can be suitable for all formaldehyde iron molybdenum catalysts, and solves the problem that the system can not continue to operate after the original iron molybdenum catalyst containing the special formula of chromium is stopped; the high-efficiency and low-consumption operation of the system is promoted, the production benefit is improved, and the production cost is reduced.
The purpose of the invention is realized by the following technical scheme:
a production method of formaldehyde comprises the steps that in the existing production method, a mixed gas is formed by preheated air at the temperature of 80-90 ℃ and methanol evaporation gas at the temperature of 70-80 ℃, the mixed gas is heated by a heating heat exchanger and then enters a reactor for reaction, and reaction gas is cooled by a cooling heat exchanger and then enters an absorption tower for absorption, and the production method is characterized in that the step of reacting the mixed gas in the reactor comprises the following steps:
1) the reactor is formed by connecting a pre-reactor, a first reactor and a second reactor in series, and the mixed gas sequentially passes through the pre-reactor, the first reactor and the second reactor;
2) the temperature of the pre-reactor is controlled to be 140-150 ℃, the temperature of the first reactor is controlled to be 150-270 ℃, and the temperature of the second reactor is controlled to be 275-425 ℃.
On the basis of the technical scheme, the following further technical scheme is provided:
the pre-reactor is internally provided with a filler with a wire mesh, so that the pre-mixing efficiency can be improved.
The first reactor and the second reactor are both filled with iron-molybdenum catalysts, and the amount of the catalysts in the second reactor is 1.5-2.5 times that in the first reactor.
The absorption tower is formed by connecting a first absorption tower, a second absorption tower and a third absorption tower in series; the absorption liquid of the first absorption tower circulates to extract finished formaldehyde, the absorption liquid of the second absorption tower circulates to extract the circulating liquid to the first absorption tower for absorption, the absorption liquid of the third absorption tower adopts desalted water for absorption, and the absorption liquid circulates to extract the circulating liquid to the second absorption tower for absorption.
The production method of formaldehyde provided by the invention has the following advantages: 1. after the method is used, formaldehyde with the content of 55% can be directly produced (the concentration of the formaldehyde produced by the production method in the prior art is 37%), the acid detection is less than or equal to 0.005%, and the methanol content is less than or equal to 0.5%; 2. all iron molybdenum catalysts can be used; 3. the high-efficiency and low-consumption operation of the system is promoted, the production benefit is improved, and the production cost is reduced.
Description of the drawings:
FIG. 1 is a flow diagram of a formaldehyde production process provided by the present invention.
The specific implementation method comprises the following steps:
example one:
the air blower is turned on, and the air quantity is controlled to be 150m3And/min, feeding fresh air, heating to 80-90 ℃ after passing through an air preheater, forming mixed gas with methanol steam at 70-80 ℃ from a methanol evaporator, raising the temperature of the mixed gas to 150 ℃ through a heating heat exchanger, fully mixing the mixed gas in a pre-reactor, heating to 140-150 ℃, controlling the concentration of methanol in the pre-reactor to be 5-8% by controlling the air flow rate and the addition of methanol, and controlling the oxygen concentration of the mixed gas and the pre-reactor to be 8.6-10.4% for safe operation of the device, so as to ensure that the oxygen concentration is below 13%, and avoid forming explosive mixtures. After the formaldehyde comes out of the pre-reactor, the formaldehyde enters a first reactor, the reaction temperature of the first reactor is 250 ℃, the mixed gas after the primary reaction enters a second reactor, the reaction temperature of the second reactor is 380 ℃, the generated gas after the reaction enters an absorption system, and is subjected to countercurrent absorption by a first absorption tower, 2 and 3 to generate finished formaldehyde from the first absorption tower, wherein the formaldehyde content in the formaldehyde is 55.02%, the acid content is 0.004% and the methanol content is 0.30% through detection; in the second reactorThe amount of the agent added was 700 kg.
Example two:
the air fan is turned on, and the air quantity is controlled to be 180m3And/min, feeding fresh air, heating to 70-80 ℃ by an air heater, mixing with 70-80 ℃ methanol steam from a methanol evaporator, raising the temperature to 150 ℃ by a heat exchanger, then fully mixing in a pre-reactor, raising the temperature to 140-150 ℃, controlling the concentration of methanol in the reactor to be 5-8% by controlling the air flow rate and the addition of methanol, and controlling the oxygen concentration of the reactor to be 8.6-10.4% for safe operation of the device, so as to ensure that the oxygen concentration is below 13%, and avoiding forming explosive mixtures. After the formaldehyde comes out of the pre-reactor, the formaldehyde enters a first reactor, the reaction temperature of the first reactor is 240 ℃, the mixed gas after the primary reaction enters a second reactor, the reaction temperature of the second reactor is 370 ℃, the generated gas after the reaction enters an absorption system, and is subjected to countercurrent absorption by a first absorption tower, 2 and 3 to generate finished formaldehyde from the first absorption tower, wherein the formaldehyde content is 54.84%, the acid content is 0.005% and the methanol content is 0.28% in the formaldehyde through detection;
the foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (2)
1. A production method of formaldehyde comprises the steps that in the existing production method, preheated air and methanol evaporation gas form mixed gas, the mixed gas enters a reactor for reaction after being heated by a heating heat exchanger, and the reaction gas enters an absorption tower for absorption after being cooled by a cooling heat exchanger, and is characterized in that the step that the mixed gas reacts in the reactor comprises the following steps:
1) the reactor is formed by connecting a pre-reactor, a first reactor and a second reactor in series, and the mixed gas sequentially passes through the pre-reactor, the first reactor and the second reactor;
2) the temperature of the pre-reactor is controlled to be 140-150 ℃, the temperature of the first reactor is controlled to be 150-270 ℃, and the temperature of the second reactor is controlled to be 275-425 ℃;
3) a filler with a wire mesh is arranged in the pre-reactor; controlling the concentration of methanol in the pre-reactor to be between 5 and 8 percent by controlling the air flow rate and the addition of the methanol, and controlling the oxygen concentration of the pre-reactor to be between 8.6 and 10.4 percent for the safe operation of the device, so as to ensure that the oxygen concentration is below 13 percent and avoid forming explosive mixtures;
4) the first reactor and the second reactor are both filled with iron-molybdenum catalysts, and the amount of the catalysts in the second reactor is 1.5-2.5 times that in the first reactor.
2. The method for producing formaldehyde according to claim 1, wherein the absorption tower comprises a first absorption tower, a second absorption tower and a third absorption tower which are connected in series; the absorption liquid of the first absorption tower circulates to extract finished formaldehyde, the absorption liquid of the second absorption tower circulates to extract the circulating liquid to the first absorption tower for absorption, the absorption liquid of the third absorption tower adopts desalted water for absorption, and the absorption liquid circulates to extract the circulating liquid to the second absorption tower for absorption.
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