CN113214055A - Methylal production process - Google Patents
Methylal production process Download PDFInfo
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- CN113214055A CN113214055A CN202110545501.8A CN202110545501A CN113214055A CN 113214055 A CN113214055 A CN 113214055A CN 202110545501 A CN202110545501 A CN 202110545501A CN 113214055 A CN113214055 A CN 113214055A
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- Prior art keywords
- methylal
- reaction
- tower
- formaldehyde
- waste water
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- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 56
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000002351 wastewater Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000605 extraction Methods 0.000 claims abstract description 5
- 239000008098 formaldehyde solution Substances 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000004821 distillation Methods 0.000 abstract description 4
- 230000002194 synthesizing effect Effects 0.000 abstract description 4
- 238000005086 pumping Methods 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 239000002386 air freshener Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- REHUGJYJIZPQAV-UHFFFAOYSA-N formaldehyde;methanol Chemical compound OC.O=C REHUGJYJIZPQAV-UHFFFAOYSA-N 0.000 description 1
- -1 good solubility Chemical compound 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/50—Preparation of compounds having groups by reactions producing groups
- C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a methylal production process, which comprises the steps of mixing methanol and 37% formaldehyde solution produced by a formaldehyde device in proportion, feeding the mixture into a heater for preheating, and pumping the mixture into a pre-reactor filled with a catalyst for pre-reaction; after the reaction is finished, transferring the reaction product into a methylal reaction tower for reaction; the sectional extraction enters an external reactor for reaction, and after the reaction is finished, the reaction product returns to the methylal reaction tower again for reaction; continuously distilling methylal, methanol, water and a small amount of formaldehyde gas generated in the reaction tower out and entering the bottom of a methylal rectifying tower; waste water at the bottom of the reaction tower is pumped into a waste water tower, and top fraction methanol, formaldehyde and the like are fed into the reaction tower again for reaction; the invention belongs to the technical field of methylal production, and particularly relates to a production process for synthesizing methylal by a continuous catalytic distillation method.
Description
Technical Field
The invention belongs to the technical field of methylal production, and particularly relates to a methylal production process.
Background
Methylal is a colorless transparent liquid with little odor, can be mixed with various reagents, is an important chemical raw material for synthesizing polyformaldehyde and the like, and is widely applied to the industries of electronic appliances, transportation, building fields, medicines, pesticides, rubber and the like. Methylal is used as an environment-friendly benzene-free solvent, and due to the unique physical and chemical properties of methylal, namely good solubility, low boiling point and good compatibility with water, the methylal can be widely applied to products such as cosmetics, household products, industrial and automobile products, insecticides, leather polishing agents, rubber industry, paints, printing ink, adhesives for shoes, electronic equipment cleaning agents, color ribbon formulas, air freshener formulas and the like, is developed rapidly in the year, and particularly shows good application development prospects in the field of aerosol.
In recent years, a sulfuric acid method has been used in a production process of methylal, and the corrosion of equipment is very serious due to the very strong corrosivity of sulfuric acid.
Disclosure of Invention
In order to solve the problems, the invention provides a production process for synthesizing methylal by a continuous catalytic distillation method.
In order to realize the functions, the technical scheme adopted by the invention is as follows: a methylal production process comprises the following steps:
1) mixing methanol and 37% formaldehyde solution produced by a formaldehyde device in proportion, and then sending the mixture into a heater to preheat the mixture to about 65 ℃; adding the mixture into a pre-reactor filled with a catalyst, and pre-reacting at 65 ℃ and 0.5 MPa;
2) after the reaction is finished, transferring the reaction product into a methylal reaction tower, and reacting at about 110 ℃ and 0.035 MPa;
3) the sectional extraction is carried out and enters an external reactor, the reaction is carried out at 65 ℃ and under 0.4MPa, and the reaction product returns to the methylal reaction tower for reaction after the reaction is finished;
4) continuously distilling methylal, methanol, water and a small amount of formaldehyde gas generated in the reaction tower out and entering the bottom of a methylal rectifying tower;
5) waste water at the bottom of the reaction tower is pumped into a waste water tower, rectification is carried out in the waste water tower at 110 ℃ and normal pressure, top fraction methanol, formaldehyde and the like enter the reaction tower again for reaction, and bottom waste water is fed into a preheater for heat exchange and then is externally used;
6) the mixed gas at the top of the reaction tower enters a methylal rectifying tower for separation, the fraction at the top of the tower is methylal, the methylal is condensed by a condenser and then is sent into a methylal intermediate tank, the purity of the methylal is analyzed and checked, the methylal is sent to a methylal storage tank if the purity is qualified, and the methylal is sent back to the rectifying tower for continuous rectification if the purity is low.
Further, the catalyst in the step 1) is a solid resin catalyst.
The invention adopts the structure to obtain the following beneficial effects: the production process of methylal provided by the invention is simple to operate, adopts a continuous catalytic distillation method to synthesize methylal, and takes methanol and formaldehyde as raw materials to react at 40-65 ℃ to generate methylal.
Drawings
FIG. 1 is a flow chart of a methylal production process of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in figure 1, the invention relates to a methylal production process, which comprises the following steps:
1) mixing methanol and 37% formaldehyde solution produced by a formaldehyde device in proportion, and then sending the mixture into a heater to preheat the mixture to about 65 ℃; adding the mixture into a pre-reactor filled with a catalyst, and pre-reacting at 65 ℃ and 0.5 MPa;
2) after the reaction is finished, transferring the reaction product into a methylal reaction tower, and reacting at about 110 ℃ and 0.035 MPa;
3) the sectional extraction is carried out and enters an external reactor, the reaction is carried out at 65 ℃ and under 0.4MPa, and the reaction product returns to the methylal reaction tower for reaction after the reaction is finished;
4) continuously distilling methylal, methanol, water and a small amount of formaldehyde gas generated in the reaction tower out and entering the bottom of a methylal rectifying tower;
5) waste water at the bottom of the reaction tower is pumped into a waste water tower, rectification is carried out in the waste water tower at 110 ℃ and normal pressure, top fraction methanol, formaldehyde and the like enter the reaction tower again for reaction, and bottom waste water is fed into a preheater for heat exchange and then is externally used;
6) the mixed gas at the top of the reaction tower enters a methylal rectifying tower for separation, the fraction at the top of the tower is methylal, the methylal is condensed by a condenser and then is sent into a methylal intermediate tank, the purity of the methylal is analyzed and checked, the methylal is sent to a methylal storage tank if the purity is qualified, and the methylal is sent back to the rectifying tower for continuous rectification if the purity is low.
The catalyst in the step 1) is a solid resin catalyst.
The process for synthesizing the methylal by adopting the continuous catalytic distillation method is adopted in the project. Methanol and formaldehyde are used as raw materials to react at 40-65 ℃ to generate methylal, and the reaction equation is shown as follows.
2CHOH+CH20 CH3OCH2OCH3+H20
When the methanol-formaldehyde mixed heating device is used specifically, a 37% formaldehyde solution produced by a methanol and formaldehyde device is mixed in proportion and then sent into a heater to be preheated to about 65 ℃; adding the mixture into a pre-reactor filled with a catalyst, and pre-reacting at 65 ℃ and 0.5 MPa; after the reaction is finished, transferring the reaction product into a methylal reaction tower, and reacting at about 110 ℃ and 0.035 MPa; the sectional extraction is carried out and enters an external reactor, the reaction is carried out at 65 ℃ and under 0.4MPa, and the reaction product returns to the methylal reaction tower for reaction after the reaction is finished; continuously distilling methylal, methanol, water and a small amount of formaldehyde gas generated in the reaction tower out and entering the bottom of a methylal rectifying tower; waste water at the bottom of the reaction tower is pumped into a waste water tower, rectification is carried out in the waste water tower at 110 ℃ and normal pressure, top fraction methanol, formaldehyde and the like enter the reaction tower again for reaction, and bottom waste water is fed into a preheater for heat exchange and then is externally used; the mixed gas at the top of the reaction tower enters a methylal rectifying tower for separation, the fraction at the top of the tower is methylal, the methylal is condensed by a condenser and then is sent into a methylal intermediate tank, the purity of the methylal is analyzed and checked, the methylal is sent to a methylal storage tank if the purity is qualified, and the methylal is sent back to the rectifying tower for continuous rectification if the purity is low.
The present invention and its embodiments have been described above, and the description is not intended to be limiting, and the drawings are only one embodiment of the present invention, and the actual structure is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (2)
1. A methylal production process is characterized by comprising the following steps:
1) mixing 37 percent formaldehyde solution produced by a methanol and formaldehyde device according to a proportion, then sending the mixture into a heater to preheat the mixture to 60-70 ℃, putting the mixture into a pre-reactor filled with a catalyst, and carrying out pre-reaction at 65 ℃ and 0.5 MPa;
2) after the reaction is finished, transferring the reaction product into a methylal reaction tower, and reacting at about 110 ℃ and 0.035 MPa;
3) the sectional extraction is carried out and enters an external reactor, the reaction is carried out at 65 ℃ and under 0.4MPa, and the reaction product returns to the methylal reaction tower for reaction after the reaction is finished;
4) continuously distilling methylal generated in the reaction tower, methanol, water and formaldehyde gas out and entering the bottom of a methylal rectifying tower;
5) waste water at the bottom of the reaction tower is pumped into a waste water tower, rectification is carried out in the waste water tower at 110 ℃ and normal pressure, top fraction methanol and formaldehyde enter the reaction tower again for reaction, and bottom waste water is fed into a feed preheater for heat exchange and then is externally used;
6) the mixed gas at the top of the reaction tower enters a methylal rectifying tower for separation, the fraction at the top of the tower is methylal, the methylal is condensed by a condenser and then is sent into a methylal intermediate tank, the purity of the methylal is analyzed and checked, the methylal is sent to a methylal storage tank if the purity is qualified, and the methylal is sent back to the rectifying tower for continuous rectification if the purity is low.
2. The process according to claim 2, wherein: the catalyst in the step 1) is a solid resin catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110545501.8A CN113214055A (en) | 2021-05-19 | 2021-05-19 | Methylal production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110545501.8A CN113214055A (en) | 2021-05-19 | 2021-05-19 | Methylal production process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113214055A true CN113214055A (en) | 2021-08-06 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110545501.8A Pending CN113214055A (en) | 2021-05-19 | 2021-05-19 | Methylal production process |
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| Country | Link |
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| CN (1) | CN113214055A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060129000A1 (en) * | 2004-12-13 | 2006-06-15 | Ticona Gmbh | Processes for the manufacture of acetals |
| CN101863746A (en) * | 2010-04-01 | 2010-10-20 | 江苏恒茂机械制造有限公司 | Dimethoxymethane production process and device thereof |
| RU2432349C1 (en) * | 2010-04-30 | 2011-10-27 | Открытое акционерное общество Научно-исследовательский институт "Ярсинтез" (ОАО НИИ "Ярсинтез") | Method of producing highly concentrated methylal |
| CN103896747A (en) * | 2014-04-08 | 2014-07-02 | 江苏凯茂石化科技有限公司 | Backpack type circulation production process device of high-concentration methylal |
| CN104193598A (en) * | 2014-08-13 | 2014-12-10 | 山东滨州新天阳化工有限责任公司 | Multi-reflux environment-friendly dimethoxymethane preparation process |
| CN104876808A (en) * | 2015-06-04 | 2015-09-02 | 中建安装工程有限公司 | Device and process for producing methylal by utilizing novel catalytic distilled and structured packing |
| CN110496576A (en) * | 2019-09-17 | 2019-11-26 | 无锡赫利邦化工科技有限公司 | A kind of synthesis of polymethoxy dimethyl ether and separation system |
-
2021
- 2021-05-19 CN CN202110545501.8A patent/CN113214055A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060129000A1 (en) * | 2004-12-13 | 2006-06-15 | Ticona Gmbh | Processes for the manufacture of acetals |
| CN101863746A (en) * | 2010-04-01 | 2010-10-20 | 江苏恒茂机械制造有限公司 | Dimethoxymethane production process and device thereof |
| RU2432349C1 (en) * | 2010-04-30 | 2011-10-27 | Открытое акционерное общество Научно-исследовательский институт "Ярсинтез" (ОАО НИИ "Ярсинтез") | Method of producing highly concentrated methylal |
| CN103896747A (en) * | 2014-04-08 | 2014-07-02 | 江苏凯茂石化科技有限公司 | Backpack type circulation production process device of high-concentration methylal |
| CN104193598A (en) * | 2014-08-13 | 2014-12-10 | 山东滨州新天阳化工有限责任公司 | Multi-reflux environment-friendly dimethoxymethane preparation process |
| CN104876808A (en) * | 2015-06-04 | 2015-09-02 | 中建安装工程有限公司 | Device and process for producing methylal by utilizing novel catalytic distilled and structured packing |
| CN110496576A (en) * | 2019-09-17 | 2019-11-26 | 无锡赫利邦化工科技有限公司 | A kind of synthesis of polymethoxy dimethyl ether and separation system |
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Application publication date: 20210806 |
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