CN113683494A - Production process of high-purity methylal - Google Patents
Production process of high-purity methylal Download PDFInfo
- Publication number
- CN113683494A CN113683494A CN202111056748.XA CN202111056748A CN113683494A CN 113683494 A CN113683494 A CN 113683494A CN 202111056748 A CN202111056748 A CN 202111056748A CN 113683494 A CN113683494 A CN 113683494A
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- China
- Prior art keywords
- methylal
- enabling
- formaldehyde
- methanol
- tower
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 81
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 75
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000004821 distillation Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000000047 product Substances 0.000 claims abstract description 10
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 8
- 239000011973 solid acid Substances 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 4
- 230000001174 ascending effect Effects 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000000630 rising effect Effects 0.000 abstract description 3
- 239000003377 acid catalyst Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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
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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 relates to a production process of high-purity methylal, which comprises the steps of enabling methanol and formaldehyde aqueous solution to enter a reactor according to a certain proportion, generating methylal under the action of a solid acid catalyst, enabling the methylal and unreacted methanol, formaldehyde and water from the reactor to enter a distillation tower under the drive of a pump, enabling a part of the methylal to circulate and further to be in contact with the catalyst to improve conversion rate and yield, enabling reaction products flowing out of each reactor to enter the distillation tower at different positions, enabling the methanol components to be high to be fed from a tower plate at the upper part, enabling the reaction products entering the distillation tower to be in contact with rising steam for mass transfer, enabling the concentration of the methylal to be gradually increased, keeping the temperature at the top of the tower at 42 ℃, enabling the products to be sent into a storage tank, and enabling the unreacted methanol, formaldehyde and water to be discharged from the bottom of the tower. The invention has the following advantages: the production efficiency is improved, the conversion rate of raw materials is high, the yield of methylal is high, the product purity is high, and the reaction period is shortened.
Description
Technical Field
The invention relates to the technical field of methylal production, in particular to a production process of high-purity methylal.
Background
The production process of methylal comprises the following steps: two molecules of methanol and one molecule of formaldehyde are subjected to condensation reaction under the action of an acid catalyst to generate one molecule of methylal, and one molecule of water is removed. A small amount of heat is released in the reaction process.
The existing methylal production process has the disadvantages of low raw material conversion rate, low methylal yield, low product purity, long reaction period and low production efficiency due to intermittent interruption of the methylal production process.
Disclosure of Invention
The invention aims to provide a production process of high-purity methylal, which aims to improve the conversion rate of raw materials and the yield of methylal, improve the product purity, shorten the reaction period and improve the production efficiency.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a production process of high-purity methylal comprises the steps of enabling methanol and formaldehyde aqueous solution to enter a reactor according to a certain ratio, generating methylal under the action of a solid acid catalyst, enabling the reaction temperature to be 45-90 ℃, enabling the methylal, unreacted methanol, formaldehyde and water to enter a distillation tower partially under the driving of a pump, enabling the methylal, the unreacted methanol, the unreacted formaldehyde and the water to circulate partially, enabling the methylal, the unreacted methanol, the unreacted formaldehyde and the water to further contact with the catalyst to improve conversion rate and yield, enabling reaction products flowing out of the reactors to enter the distillation tower at different positions, enabling the methanol components to be high to be fed from a tower plate at the upper part, enabling the reaction products entering the distillation tower to contact with rising steam to carry out mass transfer, enabling the concentration of the methylal to be gradually increased, keeping the temperature at the top of the tower at 42 ℃, enabling the products to be sent into a storage tank, and enabling the unreacted methanol, the formaldehyde and the water to be discharged from the bottom of the tower, wherein the reaction equation is as follows:
2CH3OH+HCHO→(CH3O)2CH2+H2O。
as an improvement: the stoichiometric ratio of methanol to formaldehyde is 1.0-1.2.
As an improvement: the operating pressure of the distillation tower is 0.1-0.3 Mpa.
The beneficial effects obtained by the invention are as follows: the reaction and distillation system can be continuously operated for a long time, and the solid acid catalyst is easily separated from the solution of unreacted methanol, formaldehyde and water and can be regenerated and used. The sieve plate is arranged in the reactor, so that the catalyst can be regenerated, converted and recovered without stopping the reactor, the production process of methylal is not interrupted, the production efficiency is improved, the conversion rate of raw materials is high, the yield of methylal is high, the product purity is high, and the reaction period is shortened.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1: a production process of high-purity methylal comprises the steps of enabling methanol and formaldehyde aqueous solution to enter a reactor according to a certain ratio, generating methylal under the action of a solid acid catalyst, enabling the reaction temperature to be 45-90 ℃, enabling the methylal, unreacted methanol, formaldehyde and water to enter a distillation tower partially under the driving of a pump, enabling the methylal, the unreacted methanol, the unreacted formaldehyde and the water to circulate partially, enabling the methylal, the unreacted methanol, the unreacted formaldehyde and the water to further contact with the catalyst to improve conversion rate and yield, enabling reaction products flowing out of the reactors to enter the distillation tower at different positions, enabling the methanol components to be high to be fed from a tower plate at the upper part, enabling the reaction products entering the distillation tower to contact with rising steam to carry out mass transfer, enabling the concentration of the methylal to be gradually increased, keeping the temperature at the top of the tower at 42 ℃, enabling the products to be sent into a storage tank, and enabling the unreacted methanol, the formaldehyde and the water to be discharged from the bottom of the tower, wherein the reaction equation is as follows:
2CH3OH+HCHO→(CH3O)2CH2+H2O。
the stoichiometric ratio of methanol to formaldehyde is 1.0-1.2.
The operating pressure of the distillation tower is 0.1-0.3 Mpa.
The raw material and public engineering consumption index of the process are compared with the domestic average level as shown in the following table:
| item | The process | Average domestic level | Remarks for note |
| Methanol consumption (ton/ton) | 0.87 | 0.88 | |
| Formaldehyde consumption | 1.02 | 1.05 | Converted into 100 percent formaldehyde |
| Electric kWh/ton | 45 | 60 | |
| Steam consumption (kg/ton) | 1200 | 1500 | |
| Water consumption (ton/ton) | 0 | 0 | |
| The product quality index wt% | 99.5 | 92 | |
| Maximum scale of single set of equipment (ton/year) | 16 | — | |
| Investment of single set of equipment (Wanyuan) | 1800 | Within 1 m of the boundary area of the workshop | |
| Direct production cost per unit product (%) | ～96.5 | 100 |
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (3)
1. A production process of high-purity methylal is characterized by comprising the following steps: methanol and formaldehyde aqueous solution are fed into a reactor according to a certain ratio, methylal is generated under the action of a solid acid catalyst, the reaction temperature is 45-90 ℃, the methylal discharged from the reactor, unreacted methanol, formaldehyde and water enter a distillation tower under the drive of a pump, part of the methylal and unreacted methanol, formaldehyde and water are circulated, the methylal is further contacted with the catalyst to improve the conversion rate and the yield, the reaction product discharged from each reactor is fed into the distillation tower at different positions, the methanol component is high, the reaction product entering the distillation tower is contacted with ascending steam to carry out mass transfer, the concentration of the methylal is gradually increased, the temperature at the top of the tower is kept at 42 ℃, the product is fed into a storage tank, the unreacted methanol, formaldehyde and water are discharged from the bottom of the tower, and the reaction equation is as follows:
2CH3OH+HCHO→(CH3O)2CH2+H2O。
2. the process according to claim 1, wherein the production of high purity methylal comprises the steps of: the stoichiometric ratio of methanol to formaldehyde is 1.0-1.2.
3. The process according to claim 1, wherein the production of high purity methylal comprises the steps of: the operating pressure of the distillation tower is 0.1-0.3 Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111056748.XA CN113683494A (en) | 2021-09-09 | 2021-09-09 | Production process of high-purity methylal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111056748.XA CN113683494A (en) | 2021-09-09 | 2021-09-09 | Production process of high-purity methylal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113683494A true CN113683494A (en) | 2021-11-23 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111056748.XA Pending CN113683494A (en) | 2021-09-09 | 2021-09-09 | Production process of high-purity methylal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113683494A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936569A (en) * | 2014-04-08 | 2014-07-23 | 江苏凯茂石化科技有限公司 | High-concentration dimethoxymethane production technology device and method |
| CN104230676A (en) * | 2014-08-13 | 2014-12-24 | 山东滨州新天阳化工有限责任公司 | Process for preparing methylal |
-
2021
- 2021-09-09 CN CN202111056748.XA patent/CN113683494A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936569A (en) * | 2014-04-08 | 2014-07-23 | 江苏凯茂石化科技有限公司 | High-concentration dimethoxymethane production technology device and method |
| CN104230676A (en) * | 2014-08-13 | 2014-12-24 | 山东滨州新天阳化工有限责任公司 | Process for preparing methylal |
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| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211123 |