CN1064346C - Direct synthesis method of dimethyl carbonate - Google Patents

Direct synthesis method of dimethyl carbonate Download PDF

Info

Publication number
CN1064346C
CN1064346C CN95120056A CN95120056A CN1064346C CN 1064346 C CN1064346 C CN 1064346C CN 95120056 A CN95120056 A CN 95120056A CN 95120056 A CN95120056 A CN 95120056A CN 1064346 C CN1064346 C CN 1064346C
Authority
CN
China
Prior art keywords
methanol
magnesium
carbon dioxide
reaction
dimethyl carbonate
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.)
Expired - Fee Related
Application number
CN95120056A
Other languages
Chinese (zh)
Other versions
CN1131660A (en
Inventor
江琦
林齐合
黄仲涛
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
South China University of Technology SCUT
Original Assignee
South China University of Technology SCUT
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by South China University of Technology SCUT filed Critical South China University of Technology SCUT
Priority to CN95120056A priority Critical patent/CN1064346C/en
Publication of CN1131660A publication Critical patent/CN1131660A/en
Application granted granted Critical
Publication of CN1064346C publication Critical patent/CN1064346C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/141Feedstock

Landscapes

  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention provides a method for synthesizing dimethyl carbonate by carbon dioxide, a potential carbon resource, as basic raw materials. Firstly, magnesium and methanol react to generate magnesium methoxide, and the carbon dioxide and the methanol are in gas liquid reaction to generate the dimethyl carbonate under the action of the magnesium methoxide. The method has the process conditions that the content of the magnesium accounts for 3% to 9% of the weight percentage of the methanol, the reaction temperature of the magnesium and the methanol is 200 DEG C, and the reaction time is one hour. The pressure of the carbon dioxide is from 10 to 50 kg/cm<2>, the temperature of the gas liquid reaction is from 120 to 200 DEG C, and the time of the gas liquid reaction is from 1 to 11 hours. The preparation method has the advantages of simple process, easy operation, single product, no secondary environmental pollution and good economical and social benefit.

Description

Direct synthesis method of dimethyl carbonate
Theinvention relates to a preparation method of an organic compound, in particular to a method for directly synthesizing dimethyl carbonate from carbon dioxide and methanol.
Carbon dioxide is both a potential carbon source and a major cause of environmental problems such as greenhouse effect. Numerous researchers have studied the comprehensive utilization of carbon dioxide. U.S. patent 3, 657, 310 entitled: synthesis of aliphatic carbonates, alkali metal salts of monomethyl carbonate are disclosed prepared by reacting carbon dioxide with an alkali metal methoxide. And then the methyl ester of methyl carbonate is prepared by the methylation of monohalogenated methane. This process has not been developed industrially because of the use of expensive and dangerous metallic sodium and highly toxic monohalogenated methane as raw materials. Another approach is U.S. patent No. 4,661,609 entitled: the co-synthesis of ethylene glycol and dimethyl carbonate, the ester exchange method disclosed, is that firstly carbon dioxide and alkylene oxide react to obtain cyclic carbonate, and then the cyclic carbonate and methanol undergo ester exchange reaction to obtain dimethyl carbonate. The method needs two-step reaction and two-step separation process, and has complex process and high preparation cost.
The invention aims to avoid the defects of the background technology and create a method for directly synthesizing dimethyl carbonate by carbon dioxide, which has the advantages of simple process, low cost and no secondary environmental pollution.
The object of the invention is achieved by the following measures:
a direct synthesis method of dimethyl carbonate is characterized in that magnesium and methanol are firstly reacted to generate magnesium methoxide, and then carbon dioxide and methanol are subjected to gas-liquid reaction to generate dimethyl carbonate under the action of the magnesium methoxide, wherein the reaction equation is as follows: the process conditions are as follows: (1) the magnesium content accounts for 3-9% of the weight of the methanol; (2) reaction temperature of magnesium with methanol: 200 ℃, reaction time: 1 hour; (3) the pressure of the carbon dioxide is 10-50 Kg/cm2(4) The reaction temperature of the gas-liquid reaction of the carbon dioxide and the methanol under the action of the magnesium methoxide is 120-200 ℃ (5) the reaction time of the gas-liquid reaction of the carbon dioxide and the methanol under the action of the magnesium methoxide is 1-11 hours, compared with the background art, the invention has the following advantages: 1. the preparation process is simple, convenient to operate, single in product and low in cost.
2. The preparation process of the invention does not produce secondary environmental pollution, has rich raw material sources and fully utilizes the potential carbon resource of carbon dioxide.
3. The invention has good industrialization prospect, the dimethyl carbonate is not only used as a methylation reagent, a carbonylation reagent and an organic synthesis intermediate, but also can be used as a novel fuel additive, can replace methyl tert-butyl ether, and has remarkable effect on improving the octane number and the oxygen content of the fuel.
Therefore, the invention has good economic benefit and social benefit.
The invention is further illustrated by the following examples:
example 1:
weighing 10 g of magnesium metal, adding the magnesium metal into an autoclave, mixing the magnesium metal with 200 ml of methanol, sealing the autoclave, reacting the mixture for 1 hour at 200 ℃, cooling the autoclave, and introducing 30 Kg/cm2Reacting the carbon dioxide gas at 180 ℃ for 5 hours, cooling, removing residual gas, distilling and separating to obtain the product, wherein the yield of the dimethyl carbonate is 16.4 percent (mol ratio) of the carbon dioxide raw material gas.
Example 2:
weighing 5 g of magnesium metal, adding the magnesium metal into an autoclave, mixing the magnesium metal with 200 ml of methanol, sealing the autoclave, reacting the mixture for 1 hour at 200 ℃, cooling the autoclave and introducing 30 Kg/cm2Reacting the carbon dioxide gas at 140 ℃ for 2 hours, cooling, removing residual gas, and obtaining a product by distillation and separation, wherein the yield of the dimethyl carbonate is 4.46 percent (mol ratio) of the carbon dioxide raw material gas.
Example 3
Weighing 13 g of magnesium metal, adding the magnesium metal into an autoclave, mixing the magnesium metal with 200 ml of methanol, sealing the autoclave, reacting the mixture for 1 hour at 200 ℃, cooling the autoclave and introducing 10 Kg/cm2Reacting the carbon dioxide gas at 200 ℃ for 8 hours, cooling, removing residual gas, and obtaining a product by distillation and separation, wherein the yield of the dimethyl carbonate is 15.9 percent (mol ratio) of the carbon dioxide raw material gas.
Example 4:
weighing 10 g of magnesium metal, adding into an autoclave and 200 ml of methanolMixing, sealing, reacting at 200 deg.C for 1 hr, cooling, and introducing 50Kg/cm2Reacting the carbon dioxide gas at 160 ℃ for 10 hours, cooling, removing residual gas, and obtaining a product by distillation and separation, wherein the yield of the dimethyl carbonate is 10.1 percent (mol ratio) of the carbon dioxide raw material gas.

Claims (1)

  1. The direct synthesis process of dimethyl carbonate features that magnesium and methanol are first reacted to produce magnesium methoxide, and then carbon dioxide and methanol are reacted under the action of magnesium methoxide to produce dimethyl carbonate, with the reaction equation as follows:
    Figure 9512005600021
    the process conditions are as follows:
    (1) the total amount of magnesium accounts for 3-9% of the weight of the methanol;
    (2) the reaction temperature of the reaction of magnesium and methanol is 2O0 ℃, and the reaction time is 1 hour;
    (3) the pressure of the carbon dioxide gas is 10-50 Kg/cm2
    (4) The reaction temperature of the gas-liquid reaction of the carbon dioxide and the methanol under the action of the magnesium methoxide is l 20-200 ℃;
    (5) the reaction time of the gas-liquid reaction of the carbon dioxide and the methanol under the action of the magnesium methoxide is 1-1 l hour.
CN95120056A 1995-11-27 1995-11-27 Direct synthesis method of dimethyl carbonate Expired - Fee Related CN1064346C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN95120056A CN1064346C (en) 1995-11-27 1995-11-27 Direct synthesis method of dimethyl carbonate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN95120056A CN1064346C (en) 1995-11-27 1995-11-27 Direct synthesis method of dimethyl carbonate

Publications (2)

Publication Number Publication Date
CN1131660A CN1131660A (en) 1996-09-25
CN1064346C true CN1064346C (en) 2001-04-11

Family

ID=5082235

Family Applications (1)

Application Number Title Priority Date Filing Date
CN95120056A Expired - Fee Related CN1064346C (en) 1995-11-27 1995-11-27 Direct synthesis method of dimethyl carbonate

Country Status (1)

Country Link
CN (1) CN1064346C (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106478421B (en) 2015-08-31 2019-09-13 亚申科技(浙江)有限公司 DMC Processes
WO2017093472A1 (en) 2015-12-02 2017-06-08 Ait Austrian Institute Of Technology Gmbh Method and device for the continuous production of organic carbonates from co2

Also Published As

Publication number Publication date
CN1131660A (en) 1996-09-25

Similar Documents

Publication Publication Date Title
US5516960A (en) Process for producing hydrocarbon fuels
ATE60046T1 (en) PROCESS FOR THE CARBONYLATION OF ALCOHOL TO CARBON ACID, IN PARTICULAR METHANOL TO ACETIC ACID.
CN108929221A (en) A kind of preparation method of n propyl propionate
CN1227839A (en) Process for low-pressure synthesis of dimethyl carbonate by carbon monoxide
US20070276151A1 (en) Method For Preparing Asymmetric Linear Carbonate
CN1064346C (en) Direct synthesis method of dimethyl carbonate
US4126752A (en) Homologation of methanol with a carbon monoxide-water mixture
CN103159591A (en) Technique of synthesizing ethanol with acetic acid
CN101328125B (en) Method for preparing diethyl carbonate by two-step coupling reaction
ES8204760A1 (en) Process for the production of a &#34;fuel grade&#34; mixture of methanol and higher alcohols
CN111072480A (en) Method for producing methyl ethyl carbonate by using ionic liquid catalysis ester exchange method
CN1544148A (en) Catalyst, preparation method thereof and method for synthesizing methyl carbonate
CN115057761A (en) Method for producing purified ethyl tert-butyl ether by reactive distillation coupled extraction distillation dividing wall tower technology
US4661619A (en) Process for the production of carboxylic acids and/or esters thereof
CN1158235C (en) Prepn of tri-and tetra-glycol methyl ether and utilization of side product polyglycol methyl ether
CN1218914C (en) Process for preparing 2H-heptafluoropropane
US4476334A (en) Methanol production method and system
CN116655484B (en) Preparation method of L-4-chloro-2-aminobutyric acid ester hydrochloride
CA1194040A (en) Process for producing ethanol
CN112125795B (en) Method for preparing adipic acid by oxidizing cyclohexane
CN114349595A (en) Method for recycling by-product of BDO (methanol to ethane) prepared by allyl alcohol method
US4490556A (en) Method for preparing bis[β-(N,N-dimethylamino)ethyl]ether
KR920001987B1 (en) Process of the preparation for acetic acid used with by-product gas of iron making
Fuller et al. A fluorine-mediated boron reducing agent—sodium tris (pentafluorophenoxy) borohydride. Preparation and reaction with selected organic compounds containing representative functional groups. Facile diastereoselective reduction of substituted cyclohexanones [1]
CN118164928A (en) Method for preparing 5-hydroxymethylfurfural by cellulose organic-inorganic two-phase continuous process

Legal Events

Date Code Title Description
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C06 Publication
PB01 Publication
C14 Grant of patent or utility model
GR01 Patent grant
C19 Lapse of patent right due to non-payment of the annual fee
CF01 Termination of patent right due to non-payment of annual fee