CN113563190A - Preparation method of dimethyl carbonate - Google Patents
Preparation method of dimethyl carbonate Download PDFInfo
- Publication number
- CN113563190A CN113563190A CN202110792451.3A CN202110792451A CN113563190A CN 113563190 A CN113563190 A CN 113563190A CN 202110792451 A CN202110792451 A CN 202110792451A CN 113563190 A CN113563190 A CN 113563190A
- Authority
- CN
- China
- Prior art keywords
- carbonate
- dimethyl carbonate
- ethylene
- preparation
- methanol
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/06—Preparation of esters of carbonic or haloformic acids from organic carbonates
- C07C68/065—Preparation of esters of carbonic or haloformic acids from organic carbonates from alkylene carbonates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The application relates to the field of dimethyl carbonate, in particular to a preparation method of dimethyl carbonate, which comprises the following steps: heating methanol at 50-60 ℃ for 5-10 min; adding dichloroethylene carbonate, ethylene carbonate and a catalyst into the heated methanol, and carrying out heat preservation reaction; and (3) after the heat preservation reaction in the step (2) is finished, obtaining the dimethyl carbonate. The raw materials in the preparation method do not contain heavy metal elements, so that the finally generated dimethyl carbonate has extremely low heavy metal content and is safe to use; the dichloroethylene carbonate is adopted as one of raw materials, the dichloroethylene carbonate is a byproduct for preparing the chloroethylene carbonate, has certain toxicity and is difficult to treat, and the dimethyl carbonate is prepared by utilizing the dichloroethylene carbonate, so that the waste utilization is realized, and the environmental protection benefit of pollution reduction is realized.
Description
Technical Field
The application relates to the field of dimethyl carbonate, in particular to a preparation method of dimethyl carbonate.
Background
Dimethyl carbonate has a wide range of applications, for example, in the fields of medicines, agricultural chemicals, synthetic materials, dyes, lubricants, etc., and can also be used as a solvent, a gasoline additive, etc.
Dimethyl carbonate prepared by the prior art often contains more heavy metal residues, and the preparation process is not environment-friendly.
Disclosure of Invention
In order to solve the problems that the existing dimethyl carbonate contains more residual heavy metals and the preparation method is not environment-friendly, the preparation method of the dimethyl carbonate is provided. The method has the advantages of waste utilization, pollution reduction, environmental protection and almost no heavy metal.
The application provides a preparation method of dimethyl carbonate, which adopts the following technical scheme:
a preparation method of dimethyl carbonate comprises the following steps:
(1) heating methanol at 50-60 ℃ for 5-10 min;
(2) adding dichloroethylene carbonate, ethylene carbonate and a catalyst into the methanol heated in the step (1), and carrying out heat preservation reaction;
(3) and (3) after the heat preservation reaction in the step (2) is finished, obtaining the dimethyl carbonate.
Further, the molar ratio of the methanol to the ethylene dichlorocarbonate in the step (2) is 2-10.
Further, the mass ratio of the dichloroethylene carbonate to the catalyst in the step (2) is 0.05-1.
Further, in the step (2), the mass ratio of the dichloroethylene carbonate to the ethylene carbonate is 1 to 4.
Further, the reaction temperature in the step (2) is 50-60 ℃.
Further, the reaction time in the step (2) is 4-8 h.
Further, the step (2) further comprises absorbing the tail gas by using diatom ooze.
Further, the catalyst is a quaternary phosphonium salt catalyst.
In summary, the present application has the following beneficial effects:
1. the raw materials for preparation do not contain heavy metal elements, so that the finally generated dimethyl carbonate has extremely low heavy metal content and is safe to use;
2. dichloroethylene carbonate is adopted as one of raw materials, the dichloroethylene carbonate is a byproduct for preparing the chloroethylene carbonate, has certain toxicity and is difficult to treat, and dimethyl carbonate is prepared by utilizing the dichloroethylene carbonate, so that the waste utilization is realized, and the environmental protection benefit of pollution reduction is realized;
3. and the diatom ooze is used for absorbing tail gas, so that the discharge of chlorine-containing substances generated in the preparation process can be reduced, and the environmental protection benefit is further increased.
Detailed Description
The present application will be described in further detail with reference to examples.
Examples
Example 1
A preparation method of dimethyl carbonate comprises the following steps:
(1) heating methanol at 50 deg.C for 10 min;
(2) adding dichloroethylene carbonate, ethylene carbonate and a quaternary phosphonium salt catalyst into the heated methanol in the step (1), carrying out heat preservation reaction for 8 hours at the temperature of 50 ℃, and absorbing tail gas by utilizing diatom ooze during the reaction;
(3) and (3) after the heat preservation reaction in the step (2) is finished, obtaining the dimethyl carbonate.
In the step (2), the molar ratio of the methanol to the ethylene dichlorocarbonate is 2;
in the step (2), the mass ratio of the ethylene dichlorocarbonate to the quaternary phosphonium salt catalyst is 0.05;
in the step (2), the mass ratio of ethylene dichlorocarbonate to ethylene carbonate is 1.
Example 2
A preparation method of dimethyl carbonate comprises the following steps:
(1) heating methanol at 55 deg.C for 8 min;
(2) adding dichloroethylene carbonate, ethylene carbonate and a quaternary phosphonium salt catalyst into the heated methanol obtained in the step (1), carrying out heat preservation reaction for 5 hours at the temperature of 55 ℃, and absorbing tail gas by utilizing diatom ooze during the reaction;
(3) and (3) after the heat preservation reaction in the step (2) is finished, obtaining the dimethyl carbonate.
In the step (2), the molar ratio of the methanol to the ethylene dichlorocarbonate is 6;
in the step (2), the mass ratio of the ethylene dichlorocarbonate to the quaternary phosphonium salt catalyst is 0.15;
in the step (2), the mass ratio of ethylene dichlorocarbonate to ethylene carbonate is 2.
Example 3
A preparation method of dimethyl carbonate comprises the following steps:
(1) heating methanol at 60 deg.C for 5 min;
(2) adding dichloroethylene carbonate, ethylene carbonate and a quaternary phosphonium salt catalyst into the heated methanol obtained in the step (1), carrying out heat preservation reaction for 4 hours at the temperature of 60 ℃, and absorbing tail gas by utilizing diatom ooze during the reaction;
(3) and (3) after the heat preservation reaction in the step (2) is finished, obtaining the dimethyl carbonate.
In the step (2), the molar ratio of the methanol to the dichloroethylene carbonate is 10;
in the step (2), the mass ratio of the ethylene dichlorocarbonate to the quaternary phosphonium salt catalyst is 1;
in the step (2), the mass ratio of ethylene dichlorocarbonate to ethylene carbonate is 4.
Example 4
A preparation method of dimethyl carbonate comprises the following steps:
(1) heating methanol at 58 deg.C for 8 min;
(2) adding dichloroethylene carbonate, ethylene carbonate and a quaternary phosphonium salt catalyst into the heated methanol obtained in the step (1), carrying out heat preservation reaction for 5 hours at the temperature of 55 ℃, and absorbing tail gas by utilizing diatom ooze during the reaction;
(3) and (3) after the heat preservation reaction in the step (2) is finished, obtaining the dimethyl carbonate.
In the step (2), the molar ratio of the methanol to the dichloroethylene carbonate is 7;
in the step (2), the mass ratio of the ethylene dichlorocarbonate to the quaternary phosphonium salt catalyst is 0.5;
in the step (2), the mass ratio of ethylene dichlorocarbonate to ethylene carbonate is 3.
Performance test
The compositions of the dimethyl carbonate prepared in examples 1 to 5 were measured, and the results are shown in the following table:
as can be seen from the table above, the dimethyl carbonate prepared by the method has extremely low heavy metal content and extremely low residual methanol, so that the concentration of the prepared finished product dimethyl carbonate reaches over 99.96 percent.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. The preparation method of the dimethyl carbonate is characterized by comprising the following steps:
(1) heating methanol at 50-60 ℃ for 5-10 min;
(2) adding dichloroethylene carbonate, ethylene carbonate and a catalyst into the methanol heated in the step (1), and carrying out heat preservation reaction;
(3) and (3) after the heat preservation reaction in the step (2) is finished, obtaining the dimethyl carbonate.
2. The method according to claim 1, wherein the molar ratio of methanol to ethylene dichlorocarbonate in the step (2) is 2 to 10.
3. The method according to claim 2, wherein the mass ratio of ethylene dichlorocarbonate to the catalyst in the step (2) is 0.05 to 1.
4. The method according to claim 2, wherein the mass ratio of ethylene dichlorocarbonate to ethylene carbonate in the step (2) is 1 to 4.
5. The method for preparing dimethyl carbonate according to claim 1, wherein the reaction temperature in the step (2) is 50 to 60 ℃.
6. The method for preparing dimethyl carbonate according to claim 1, wherein the reaction time in the step (2) is 4-8 h.
7. The method for preparing dimethyl carbonate according to claim 1, wherein the step (2) further comprises absorbing the tail gas by using diatom ooze.
8. The method for producing dimethyl carbonate according to any one of claims 1 to 7, wherein the catalyst is a quaternary phosphonium salt catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110792451.3A CN113563190A (en) | 2021-07-14 | 2021-07-14 | Preparation method of dimethyl carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110792451.3A CN113563190A (en) | 2021-07-14 | 2021-07-14 | Preparation method of dimethyl carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113563190A true CN113563190A (en) | 2021-10-29 |
Family
ID=78164695
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110792451.3A Pending CN113563190A (en) | 2021-07-14 | 2021-07-14 | Preparation method of dimethyl carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113563190A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20040034183A (en) * | 2002-10-21 | 2004-04-28 | 한국과학기술연구원 | Process for preparing dimethyl carbonate using K/MgO catalyst |
| CN102126957A (en) * | 2011-01-11 | 2011-07-20 | 中国科学院过程工程研究所 | Method for preparing carbonic ester and ethylene alcohol by ionic liquid catalysis |
| CN105272858A (en) * | 2014-07-24 | 2016-01-27 | 中国石油化工股份有限公司 | Dimethyl carbonate production method |
| CN108404978A (en) * | 2018-03-02 | 2018-08-17 | 中国海洋石油集团有限公司 | A kind of purposes of alkane base quaternary alkylphosphonium salt as catalyst carbonate synthesis binary esters |
| CN112624925A (en) * | 2020-12-27 | 2021-04-09 | 江苏瀚康新材料有限公司 | Method for preparing dimethyl carbonate by using waste |
-
2021
- 2021-07-14 CN CN202110792451.3A patent/CN113563190A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20040034183A (en) * | 2002-10-21 | 2004-04-28 | 한국과학기술연구원 | Process for preparing dimethyl carbonate using K/MgO catalyst |
| CN102126957A (en) * | 2011-01-11 | 2011-07-20 | 中国科学院过程工程研究所 | Method for preparing carbonic ester and ethylene alcohol by ionic liquid catalysis |
| CN105272858A (en) * | 2014-07-24 | 2016-01-27 | 中国石油化工股份有限公司 | Dimethyl carbonate production method |
| CN108404978A (en) * | 2018-03-02 | 2018-08-17 | 中国海洋石油集团有限公司 | A kind of purposes of alkane base quaternary alkylphosphonium salt as catalyst carbonate synthesis binary esters |
| CN112624925A (en) * | 2020-12-27 | 2021-04-09 | 江苏瀚康新材料有限公司 | Method for preparing dimethyl carbonate by using waste |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108452640B (en) | Ternary eutectic solvent | |
| CN102796600B (en) | Preparation method of high-grade borate type automobile brake fluid | |
| CN107674195B (en) | Catalyst for synthesizing polyethylene oxide polymer and synthesis method thereof | |
| CN103724201A (en) | Method for preparing ethyl levulinate by catalyzing biomass sugar to be directly alcoholyzed | |
| CN102965669B (en) | Method for preparing water-soluble high-temperature corrosion inhibitor | |
| CN101168493B (en) | Preparation method for fluorochlorobenzene | |
| CN110872254B (en) | Pyrazole salt diionic liquid and method for catalytic synthesis of cyclic carbonate by using same | |
| CN113563190A (en) | Preparation method of dimethyl carbonate | |
| CN103073426A (en) | Preparation process for catalyzing and synthesizing tert-butyl acrylate by using strong acid cation exchange resin as catalyst | |
| CN106145395B (en) | A kind of water soluble dispersing agent and its application | |
| CN107501526B (en) | DOPO type epoxy resin curing agent and preparation method thereof | |
| CN109504560A (en) | A kind of safe and efficient paraffin removal agent for carbon hydrogen detergent and preparation method thereof | |
| CN113663710B (en) | Magnetic solid acid catalyst and application thereof in catalyzing fructose hydrolysis reaction | |
| CN113582861A (en) | Preparation method of gemini polyhydroxy quaternary ammonium salt modified rosin surfactant | |
| CN109678725B (en) | Process for preparing p-phenylenediamine | |
| CN110510608B (en) | Antioxidant for improving oxidation resistance of flake graphite and application thereof | |
| CN103394371A (en) | Method for producing vinyl-4-hydroxybutyl ether through acetylene method, and catalyst thereof | |
| CN111303961A (en) | Recycled ester, preparation method thereof and application thereof in preparation of HZY3 brake fluid | |
| CN114621468B (en) | Synthesis method of chlorine-free environment-friendly toughening diluent | |
| CN1847234B (en) | Tetrahydro furfuryl alcohol preparing process | |
| CN105037192A (en) | One-step method for synthesizing p-formylamino benzene alkyl ether as octane booster | |
| CN102408454A (en) | Method for synthesizing metallocene carbonyl derivative | |
| CN115781843B (en) | Water-based flame retardant treating agent and preparation method thereof | |
| CN108976390B (en) | High-transparency yellowing-resistant epoxy resin curing accelerator and preparation method thereof | |
| CN110372740B (en) | Method for preparing trimethylchlorosilane from dimethylchlorosilane |
Legal Events
| 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 |