CN104710292B - A kind of process for purification and process unit of anhydrous pure formaldehyde gas - Google Patents
A kind of process for purification and process unit of anhydrous pure formaldehyde gas Download PDFInfo
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- CN104710292B CN104710292B CN201510128447.1A CN201510128447A CN104710292B CN 104710292 B CN104710292 B CN 104710292B CN 201510128447 A CN201510128447 A CN 201510128447A CN 104710292 B CN104710292 B CN 104710292B
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- tower
- assistant agent
- formaldehyde gas
- anhydrous
- formaldehyde
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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
- C07C45/85—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to a chemical modification
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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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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of process for purification and process unit of anhydrous pure formaldehyde gas, the technique is introduced a kind of water insoluble and not reacted with water, and the assistant agent for only being reacted with formaldehyde, the assistant agent reacts with formalin and obtains hemiacetal reactant, the hemiacetal reactant is water insoluble, and the small heat-sensitive substance of density ratio water, back reaction decomposition is susceptible under the too high environment of temperature, pure formaldehyde gas and liquid adjuvants are obtained by heat resolve.Present invention process is simple, energy consumption is low, simple to operate, and effect on environment is smaller.
Description
Technical field
The invention belongs to chemical production technology and equipment technical field, relate generally to anhydrous formaldehyde gas process for purification and
Process equipment.
Background technology
Formaldehyde is a most important downstream product of methyl alcohol, and methyl alcohol is an important downstream product of coal.Cause
This formaldehyde turns into the important development branch in one, derived energy chemical field.Formaldehyde is the raw material of various chemical products, in the market
It is many to exist in the form of 37% formalin.The presence of a large amount of water is not only impacted to some quality of chemical products, but also
The reaction of correlation can be influenceed, a large amount of unnecessary accessory substances is caused or is caused the low problem of conversion ratio.Dehydration simultaneously brings again
The problem of high energy consumption, therefore a large amount of presence of water limit the use face of formaldehyde.
To obtain water-free pure gas formaldehyde, usually using the concentration of formalin, subtracted by formalin
The method synthesis of solid formaldehyde or synthesizing triformol of distillation are pressed, then by trimerization and poly by high-temperature heating, parses it
Go out pure formaldehyde monomers.Complex process, it is relatively costly.
The content of the invention
Goal of the invention：For above-mentioned problem and defect, the invention provides a kind of essence of anhydrous pure formaldehyde gas
Method processed and process unit, the process is simple of the formaldehyde gas process for purification, energy consumption are low, simple to operate, and effect on environment is more
It is small.
Technical scheme：For achieving the above object, the present invention uses following technical scheme：A kind of anhydrous pure formaldehyde gas
Process for purification, comprises the following steps：
（1）Formalin is passed through at the top of packed tower, filler tower bottom is then passed through assistant agent so that formalin with
Assistant agent is inversely contacted between filler plate, concurrent biochemical reaction, obtains density less than water and water insoluble upper strata hemiacetal
Class reactant；The temperature of described filler tower is 50~100 DEG C, and assistant agent and the feed rate ratio of formalin are 1~5:1；
（2）By step（1）Obtain further rectification under vacuum, removing in the hemiacetal class reactant feeding vacuum rectification tower of upper strata
Remaining moisture, obtains anhydrous hemiacetal reactant；
（3）Anhydrous hemiacetal reactant feeding formaldehyde monomers depart from heat resolve in tower, and pure formaldehyde gas is obtained from tower top
Body, the assistant agent that bottom of towe is regenerated.
Preferably, the assistant agent monohydric alcohol or dihydroxylic alcohols.
Preferably, the assistant agent is unitary saturated alcohols or binary saturated alcohols.
Preferably, the assistant agent is one or more in isobutanol, 4- methyl -2- amylalcohols or cyclohexanol of mixture.
Preferably, the formalin is 37~85%.
Preferably, the reaction pressure in the vacuum rectification tower is -0.06MPa- normal pressures, temperature is 110~150 DEG C.
Preferably, the temperature that the formaldehyde monomers depart from tower is 150~250 DEG C, pressure is normal pressure -0.4MPa.
Present invention also offers the anhydrous pure formaldehyde gas process for refining device of one kind, including Reaction Separation packed tower, decompression
Rectifying column and formaldehyde monomers depart from tower, wherein：The Reaction Separation packed tower includes conversion zone and segregation section, and wherein conversion zone is
Packing section, the top of packing section is provided with formalin entrance, and bottom is provided with assistant agent entrance；The segregation section is that diameter is relative to be filled out
Expect the expanding reach of Duan Geng great（Enable in the hemiacetal reactant floating-upward process that conversion zone reaction is obtained into expanding reach
Speed is produced and slowed down, the moisture for being conducive to deposition to carry）, and be located on conversion zone；The Reaction Separation packed tower segregation section
Top tower departed from vacuum rectification tower and formaldehyde monomers by pipeline and liquid pump be successively connected；The formaldehyde monomers depart from tower
Outlet at bottom forms circulation with the assistant agent entrance of Reaction Separation packed tower by pipeline and liquid pump, and top is then provided with formaldehyde gas
Extraction mouth.
Beneficial effect：Compared with prior art, present invention process is simple, and energy consumption is low, and is separated using conventional rectifying
Equipment, it is simple to operate.Successfully solve conventional paraformaldehyde and metaformaldehyde synthesis high cost, the defect of complex process.Poly
Formaldehyde is solid with metaformaldehyde, and production and transport has certain dust pollution, has certain nocuity to environment and personnel.
Brief description of the drawings
Fig. 1 is the structural representation of anhydrous formaldehyde process for refining device of the present invention.
Wherein, Reaction Separation packed tower 1, vacuum rectification tower 2, formaldehyde monomers depart from tower 3, conversion zone 4, segregation section 5, used heat
Retracting device 6.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate
The present invention rather than limitation the scope of the present invention, after the present invention has been read, those skilled in the art are to of the invention each
The modification for planting the equivalent form of value falls within the application appended claims limited range.
As shown in figure 1, preheated to 50-100 DEG C of 37%-85% formalins are pumped into extraction tower top, fresh assistant agent and
Circulation assistant agent pumps into extraction tower bottom together, and feeding temperature is controlled at 50-100 DEG C, is isobutanol, 4- first as preferred assistant agent
Base -2- amylalcohols and cyclohexanol equally can also play identical function.Both concurrent biochemical reactions of the counter current contacting in packed tower tower
Hemiacetal reactant is obtained, the product density is similarly less than water.Therefore tower top obtains the light reactant of density, and content of formaldehyde
It is 15-30% or so, and by the deceleration of tower top expanding reach in the presence of deposition fraction water so that tower top water content exists
In the range of 1-6%；Packed tower bottom of towe is then dilute formalin of 5-15%, can be used for synthesizing dimethoxym ethane or as Formaldehyde Production
The moisturizing of device.Wherein, 50 DEG C -100 DEG C of the operation temperature of Reaction Separation packed tower, pressure is normal pressure -0.2MPa, assistant agent and first
The feed rate ratio of aldehyde solution is 1-5:1, preferably 3:1.Then filler tower top upper strata is contained by a small amount of water by liquid pump
The hemiacetal reactant feeding vacuum rectification tower divided, further purification, the moisture of removal remnants, 110 DEG C -150 DEG C of operation temperature,
Pressure is -0.06MPa- normal pressures.Finally, refining reaction thing enters formaldehyde monomers and departs from tower, by high temperature section, hemiacetal reactant
Decompose reaction, obtain formaldehyde monomers and assistant agent, assistant agent is regenerated, recycle.Formaldehyde monomers depart from tower operation temperature
150 DEG C -250 DEG C, pressure is normal pressure -0.4MPa.
Principle of the invention is：Introduce a kind of water insoluble and do not react with water, and the assistant agent for only being reacted with formaldehyde, should
Assistant agent reacts with formalin and obtains hemiacetal reactant, and the hemiacetal reactant is water insoluble, and density ratio water is small, weight
What is wanted is that hemiacetal reactant is a kind of heat-sensitive substance, and back reaction decomposition is susceptible under the too high environment of temperature, is obtained
Pure formaldehyde gas and liquid adjuvants, and assistant agent realizes recycling, while can also be by the waste heat of the assistant agent of high temperature by useless
Heat reclamation device is recycled.
Present invention process is simple, and energy consumption is low, and using conventional rectifying separation equipment, it is simple to operate.Successfully solve
Conventional paraformaldehyde and metaformaldehyde synthesis high cost, the defect of complex process.Paraformaldehyde is solid with metaformaldehyde, raw
Producing transport has certain dust pollution, has certain nocuity to environment and personnel.
Claims (7)
1. a kind of anhydrous pure formaldehyde gas process for purification, it is characterised in that comprise the following steps：
(1) formalin is passed through at the top of packed tower, filler tower bottom is then passed through assistant agent so that formalin and assistant agent
Inversely contacted between filler plate, concurrent biochemical reaction obtains density less than water and water insoluble upper strata hemiacetal class is anti-
Answer thing；The temperature of described filler tower is 50~100 DEG C, and assistant agent and the feed rate ratio of formalin are 1~5:1；
(2) step (1) is obtained into further rectification under vacuum in upper strata hemiacetal class reactant feeding vacuum rectification tower, removing is remaining
Moisture, obtain anhydrous hemiacetal reactant；
(3) anhydrous hemiacetal reactant feeding formaldehyde monomers depart from heat resolve in tower, and pure formaldehyde gas, tower are obtained from tower top
The assistant agent that bottom is regenerated；
The anhydrous pure formaldehyde gas process for refining device includes that Reaction Separation packed tower, vacuum rectification tower and formaldehyde monomers depart from
Tower, wherein：
The Reaction Separation packed tower includes conversion zone and segregation section, and wherein conversion zone is packing section, and the top of packing section is provided with
Formalin entrance, and bottom is provided with assistant agent entrance；The segregation section is the diameter expanding reach bigger with respect to packing section, and is located at
On conversion zone；
The top of the Reaction Separation packed tower segregation section is de- with vacuum rectification tower and formaldehyde monomers successively by pipeline and liquid pump
From tower connection；The assistant agent entrance of outlet at bottom and Reaction Separation packed tower that the formaldehyde monomers depart from tower passes through pipeline and liquid pump
Circulation is formed, and top is then provided with formaldehyde gas extraction mouth.
2. anhydrous pure formaldehyde gas process for purification according to claim 1, it is characterised in that：The assistant agent is monohydric alcohol or two
First alcohol.
3. anhydrous pure formaldehyde gas process for purification according to claim 2, it is characterised in that：The assistant agent is unitary saturated alcohols
Or binary saturated alcohols.
4. anhydrous pure formaldehyde gas process for purification according to claim 3, it is characterised in that：The assistant agent is isobutanol, 4-
One or more of mixture in methyl -2- amylalcohols or cyclohexanol.
5. anhydrous pure formaldehyde gas process for purification according to claim 1, it is characterised in that：The formalin be 37~
85%.
6. anhydrous pure formaldehyde gas process for purification according to claim 1, it is characterised in that：It is anti-in the vacuum rectification tower
Pressure is answered for -0.06MPa- normal pressures, temperature is 110~150 DEG C.
7. anhydrous pure formaldehyde gas process for purification according to claim 1, it is characterised in that：The formaldehyde monomers depart from tower
Temperature is 150~250 DEG C, and pressure is normal pressure -0.4MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510128447.1A CN104710292B (en) | 2015-03-24 | 2015-03-24 | A kind of process for purification and process unit of anhydrous pure formaldehyde gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510128447.1A CN104710292B (en) | 2015-03-24 | 2015-03-24 | A kind of process for purification and process unit of anhydrous pure formaldehyde gas |
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| Publication Number | Publication Date |
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| CN104710292A CN104710292A (en) | 2015-06-17 |
| CN104710292B true CN104710292B (en) | 2017-06-06 |
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| CN201510128447.1A Expired - Fee Related CN104710292B (en) | 2015-03-24 | 2015-03-24 | A kind of process for purification and process unit of anhydrous pure formaldehyde gas |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353188A (en) * | 2016-05-10 | 2017-11-17 | 北京旭阳科技有限公司 | A kind of method for preparing anhydrous gaseous formaldehyde |
| CN107285999A (en) * | 2017-07-13 | 2017-10-24 | 湖北三里枫香科技有限公司 | A kind of alkyl polyoxyether DMMn reaction tower and manufacturing technique method |
| CN112898145A (en) * | 2021-03-22 | 2021-06-04 | 邢台旭阳科技有限公司 | Gas-phase formaldehyde extraction system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3423368A (en) * | 1965-10-14 | 1969-01-21 | Hary E Cier | Extractive recovery of formaldehyde |
| NL6814946A (en) * | 1968-10-18 | 1970-04-21 | Recovery of formaldehyde from aqueous formaldehyde - streams | |
| CN103339094A (en) * | 2011-01-26 | 2013-10-02 | 宝理塑料株式会社 | Method for producing hemiformal concentrate and method for producing formaldehyde gas |
-
2015
- 2015-03-24 CN CN201510128447.1A patent/CN104710292B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3423368A (en) * | 1965-10-14 | 1969-01-21 | Hary E Cier | Extractive recovery of formaldehyde |
| NL6814946A (en) * | 1968-10-18 | 1970-04-21 | Recovery of formaldehyde from aqueous formaldehyde - streams | |
| CN103339094A (en) * | 2011-01-26 | 2013-10-02 | 宝理塑料株式会社 | Method for producing hemiformal concentrate and method for producing formaldehyde gas |
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| CN104710292A (en) | 2015-06-17 |
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