CN1683326A - Process for producing methyl carbamate - Google Patents
Process for producing methyl carbamate Download PDFInfo
- Publication number
- CN1683326A CN1683326A CN 200510042482 CN200510042482A CN1683326A CN 1683326 A CN1683326 A CN 1683326A CN 200510042482 CN200510042482 CN 200510042482 CN 200510042482 A CN200510042482 A CN 200510042482A CN 1683326 A CN1683326 A CN 1683326A
- Authority
- CN
- China
- Prior art keywords
- reaction
- urea
- urethylane
- methyl alcohol
- 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.)
- Granted
Links
Abstract
The methyl carbamate producing process belongs to the field of fine chemical technology. The technological scheme of purifying methyl carbamate includes: dissolving urea in methanol to obtain methanol solution of urea of 0.01-10 mol/L concentration, reaction in reactor at 100-180 deg.c and 0.1-1.5 MPa for 0.5-10 hr, condensing in condensator to separate ammonia and making ammonia produce ammonia water, returning methanol with ammonia separated to the reaction system, and product purification. The present invention has high methyl carbamate yield, simplified operation, short reaction period, low power consumption and low cost.
Description
One, technical field
The invention belongs to a kind of technical process of producing Urethylane, belong to fine chemistry industry production technique field.
Two, background technology
Urethylane (Met hour yl Carbamate is called for short MC), another name urethylan (Ureat hour ylane), methyl Wu Laitan (Met hour yluret hour ane) are a kind of important organic synthesis intermediates.Be mainly used in the synthetic of medicine, agricultural chemicals, its derivative obtains application more and more widely as weedicide, sterilant, rubber antioxygen, thermo-stabilizer etc. at agricultural, rubber industry.Carbamate chemicals for agriculture, since it with the agricultural chemicals of other kind compare people and other Mammals have low toxicity, poisoning specificity by force, easily by multiple factor degrade, residual low, to characteristics such as the side effect of environment are little, develop novel pesticide, weedicide and kill mosquito faster, fly agent so become countries in the world in recent years, and its Application Areas is expanded very fast.
The present existing MC synthetic production technique in home and abroad mainly adopts phosgene route, owing to produce raw materials used all poisonously with solvent, so complex process is very high to the equipment requirements condition, investment is huge, production cost is very high.The existing alcoholysis of urea technological process of production has also caused the complicated of technical process because of the separation that comprises various catalyzer, processing etc., because of catalyst system therefor equipment is had corrodibility simultaneously, and equipment material is had relatively high expectations, thereby has caused facility investment bigger.
Three, summary of the invention
The objective of the invention is defective, a kind of catalyst-free is provided, is the production technique of raw material homogeneous reaction production Urethylane with urea and methyl alcohol at the prior art existence.
Technical scheme of the present invention is to be raw material with urea and methyl alcohol, the production technique of producing Urethylane comprises that mainly material dissolution, reaction are synthesized, operation totally enclosed circulating reaction flow processs such as methyl alcohol, ammoniacal liquor formation are reclaimed in rectifying, production equipment mainly comprises reactor, rectifying tower, the ammoniacal liquor generating apparatus.
Technical process of the present invention is as follows:
With methyl alcohol, urea in 1～20: the dissolving of 1 ratio, making the urea concentration of methanol solution is 0.01～10mol/L, join reactor, in temperature of reaction is 100～180 ℃, reaction pressure is to react 0.5～10 hour under the condition of 0.1～1.5Mpa, to after condenser condenses, isolate reaction system by the resultant ammonia that the methyl alcohol of one of reactant is taken out of through rectifying tower in the reaction process, and enter the ammoniacal liquor generation system and generate ammoniacal liquor.Simultaneously the methyl alcohol that separates behind the N hours 3 of rectifying tower returns the reaction system recycle.After reaction finishes reaction solution being carried out product purifies.
The invention has the advantages that: this technical process has realized with urea and methyl alcohol being the operation of raw material homogeneous reaction suitability for industrialized production Urethylane, increasing rectifying tower on reactor can make the ammonia that reacts generation break away from the synthetic system of reactor effectively, impel in the synthetic system urea to the conversion of Urethylane, improved the productive rate of Urethylane greatly, simplify schedule of operation, shortened the reaction times.The material balance of whole process flow, energy exchange balance are controlled the highly selective that has realized product by reaction conditions, have reached rational comprehensive utilization, have reduced raw material and energy expenditure, have saved production cost greatly.
Four, description of drawings: do not have.
Five, embodiment
Embodiment 1: urea and methyl alcohol pro rata magnitude relation are joined in the reactor, and 140 ℃ of reacting by heating temperature are opened reactor gas phase and rectifying tower connecting tube valve when pressure reaches 1.5Mpa, and rectifying tower is started working, with 0.2m
3It is the urea methanol solution of 1mol/L that/hour speed is replenished concentration, and the control reactor is to the gas phase rate of release of rectifying tower, with keep material in the reactor into and out of material balance, 4 hours reaction times.The Urethylane productive rate is 86%.While by-product 30% ammoniacal liquor.
Embodiment 2: urea and methyl alcohol pro rata magnitude relation are joined in the reactor, and 150 ℃ of reacting by heating temperature are opened reactor gas phase and rectifying tower connecting tube valve when pressure reaches 1.0Mpa, and rectifying tower is started working, with 0.5m
3/ hour speed is replenished the urea methanol solution of concentration 0.5mol/L, and the control reactor is to the gas phase rate of release of rectifying tower, with keep material in the reactor into and out of material balance, 3 hours reaction times.The Urethylane productive rate is 90%.While by-product 30% ammoniacal liquor.
Embodiment 3:
Urea and methyl alcohol pro rata magnitude relation are joined in the reactor, and 150 ℃ of reacting by heating temperature are opened reactor gas phase and rectifying tower connecting tube valve when pressure reaches 1.5Mpa, and rectifying tower is started working, with 0.2m
3/ hour speed is replenished the urea methanol solution of concentration 1.5mol/L, and the control reactor is to the gas phase rate of release of rectifying tower, with keep material in the reactor into and out of material balance, 4 hours reaction times.The Urethylane productive rate is 88%.While by-product 30% ammoniacal liquor.
Embodiment 4:
Urea and methyl alcohol pro rata magnitude relation are joined in the reactor, and 160 ℃ of reacting by heating temperature are opened reactor gas phase and rectifying tower connecting tube valve when pressure reaches 1.0Mpa, and rectifying is started working, with 1.0m
3/ hour speed is replenished the urea methanol solution of concentration 1.2mol/L, and the control reactor is to the gas phase rate of release of rectifying tower, with keep material in the reactor into and out of material balance, 3 hours reaction times.The Urethylane productive rate is 91%.While by-product 30% ammoniacal liquor.
Embodiment 5:
Urea and methyl alcohol pro rata magnitude relation are joined in the reactor, heating, 175 ℃ of temperature of reaction are opened reactor gas phase and rectifying tower connecting tube valve when pressure reaches 1.5Mpa, and rectifying tower is started working, with 0.05m
3It is the urea methanol solution of 1mol/L that/hour speed is replenished concentration, and the control reactor is to the gas phase rate of release of rectifying tower, with keep material in the reactor into and out of material balance, 2 hours reaction times.The Urethylane productive rate is 89%.While by-product 30% ammoniacal liquor.
Claims (5)
1, a kind of technology of producing Urethylane is characterized in that comprising
Material dissolution: with urea and methyl alcohol is raw material, and by urea: the ratio of the weight of methyl alcohol is to mix at 1～20: 1, and mixed urea concentration of methanol solution is 0.01～10mol/L;
Reaction is synthetic: mixed urea methanol solution reacted 0.5～10 hour under the condition of 100～180 ℃ of temperature of reaction, reaction pressure 0.1～1.5Mpa;
Product is purified: after reaction finishes reaction solution is carried out product and purify.
2, the technology of production Urethylane according to claim 1 is characterized in that also comprising Methanol Recovery: the ammonia that discharges in the reaction process-methanol mixed steam goes out ammonia gas and methyl alcohol by rectifying separation, and methyl alcohol reclaims after cooling off.
3, the technology of production Urethylane according to claim 2 is characterized in that isolating ammonia gas and isolate methyl alcohol once more, Methanol Recovery after cooling in the Methanol Recovery process.
4, the technology of production Urethylane according to claim 2 is characterized in that material dissolution realizes by the pre-mixing still; Reaction is synthetic to be to carry out in the totally enclosed reactor that has an agitator; It is to carry out in separating still that product is purified; Methanol Recovery realizes by essence slide tower, water cooler.
5, the technology of production Urethylane according to claim 1, it is characterized in that: in reaction is synthetic, pass through the burst size of control ammonia gas and the additional speed of urea methanol solution, realize suppressing urea decomposition, impel molecular balance to move to generating the Urethylane direction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100424828A CN100357266C (en) | 2005-02-21 | 2005-02-21 | Process for producing methyl carbamate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100424828A CN100357266C (en) | 2005-02-21 | 2005-02-21 | Process for producing methyl carbamate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1683326A true CN1683326A (en) | 2005-10-19 |
| CN100357266C CN100357266C (en) | 2007-12-26 |
Family
ID=35262853
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100424828A Expired - Fee Related CN100357266C (en) | 2005-02-21 | 2005-02-21 | Process for producing methyl carbamate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100357266C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101570499A (en) * | 2009-03-07 | 2009-11-04 | 垦利三合新材料科技有限责任公司 | Method for preparing methyl carhamate |
| CN101781202A (en) * | 2009-01-16 | 2010-07-21 | 亚申科技研发中心（上海）有限公司 | Reaction process and system for preparing organic carbonic ester by catalytic alcoholysis of urea |
| CN103254101A (en) * | 2013-04-03 | 2013-08-21 | 中北大学 | Method and equipment for preparation of methyl carbamate |
| CN106631901A (en) * | 2016-12-14 | 2017-05-10 | 中榆化工科技有限公司 | Method for preparing methyl carbamate by urea alcoholysis method and device thereof |
| CN113651751A (en) * | 2021-09-28 | 2021-11-16 | 大连九信精细化工有限公司 | Preparation method of N-methoxycarbonyl-3-trifluoromethylpyridine-2-sulfonamide |
| CN114656375A (en) * | 2022-05-06 | 2022-06-24 | 山东禹城易澳科技有限公司 | Methyl carbamate refining process |
| CN114956119A (en) * | 2022-04-26 | 2022-08-30 | 山东禹城易澳科技有限公司 | Method for treating distillation residue of carbamate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3881386B2 (en) * | 1994-10-21 | 2007-02-14 | 多摩化学工業株式会社 | Process for producing dialkyl carbonate |
| CN1241908C (en) * | 2003-07-11 | 2006-02-15 | 中国科学院山西煤炭化学研究所 | Method of synthesizing methyl carbamate |
-
2005
- 2005-02-21 CN CNB2005100424828A patent/CN100357266C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781202A (en) * | 2009-01-16 | 2010-07-21 | 亚申科技研发中心（上海）有限公司 | Reaction process and system for preparing organic carbonic ester by catalytic alcoholysis of urea |
| CN101781202B (en) * | 2009-01-16 | 2014-04-23 | 亚申科技研发中心（上海）有限公司 | Reaction process and system for preparing organic carbonic ester by catalytic alcoholysis of urea |
| CN101570499A (en) * | 2009-03-07 | 2009-11-04 | 垦利三合新材料科技有限责任公司 | Method for preparing methyl carhamate |
| CN103254101A (en) * | 2013-04-03 | 2013-08-21 | 中北大学 | Method and equipment for preparation of methyl carbamate |
| CN103254101B (en) * | 2013-04-03 | 2015-12-23 | 中北大学 | Prepare the method and apparatus of Urethylane |
| CN106631901A (en) * | 2016-12-14 | 2017-05-10 | 中榆化工科技有限公司 | Method for preparing methyl carbamate by urea alcoholysis method and device thereof |
| CN106631901B (en) * | 2016-12-14 | 2019-02-05 | 中榆化工科技有限公司 | A kind of method and device thereof preparing methyl carbamate using alcoholysis of urea |
| CN113651751A (en) * | 2021-09-28 | 2021-11-16 | 大连九信精细化工有限公司 | Preparation method of N-methoxycarbonyl-3-trifluoromethylpyridine-2-sulfonamide |
| CN114956119A (en) * | 2022-04-26 | 2022-08-30 | 山东禹城易澳科技有限公司 | Method for treating distillation residue of carbamate |
| CN114656375A (en) * | 2022-05-06 | 2022-06-24 | 山东禹城易澳科技有限公司 | Methyl carbamate refining process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100357266C (en) | 2007-12-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100357266C (en) | Process for producing methyl carbamate | |
| CN103922931B (en) | A kind of method of a step catalytically synthesizing glycol ether acetate | |
| CN102786499B (en) | Method for preparing cyclohexene oxide | |
| CN110078702A (en) | A kind of method of poly ion liquid frame catalyst preparation cyclic carbonate | |
| CN102060837B (en) | Preparation method of cyclic carbonic ester | |
| CN102040561A (en) | Method for synthesizing benzotriazole ultraviolet absorber | |
| CN100415712C (en) | Process for producing methyl carbamate by low pressure solvation homogeneous phase reaction | |
| CN109675631B (en) | Catalyst for preparing glycol by hydrating epoxy compound and application thereof | |
| CN103709010B (en) | A kind of by tetrahydrobenzene, carboxylic acid and water Reactive Synthesis hexalin method | |
| CN101372445B (en) | Resorcin synthetic process | |
| CN106831595B (en) | A kind of benzyl imidazole ionic liquid and the method using its catalytically synthesizing cyclic carbonate ester | |
| CN102786500B (en) | Preparation method of cyclohexene oxide | |
| CN102755910A (en) | Titanium silicon molecular sieve and resin composite modified catalyst and preparation method thereof | |
| CN111393402B (en) | N & lt/EN & gt acid/quaternary ammonium salt composite catalytic CO 2 Method for preparing cyclic carbonate by cycloaddition with epoxide | |
| CN103534231B (en) | Prepare the method for polymethylene polyphenyl polyamino formate | |
| CN101456792A (en) | Method for preparing diatomic alcohol compounds by annular carbonic acid esters hydrolysis | |
| CN103252239B (en) | Catalyst for synthesizing glycerol carbonic, preparation method for catalyst and application of catalyst | |
| CN114315749B (en) | Method for synthesizing aliskiren intermediate by continuous flow microreactor | |
| CN101781202A (en) | Reaction process and system for preparing organic carbonic ester by catalytic alcoholysis of urea | |
| CN110885286B (en) | Preparation method of alpha-isophorone | |
| CN1569806A (en) | Process for synthesizing carbonic ethenyl (allyl) ester from carbon dioxide and epoxy ethane (propane) | |
| CN109232213A (en) | The method of hydroxy pivalin aldehyde is prepared under a kind of super critical condition | |
| CN102942479A (en) | Method for preparing propylene glycol methyl ether acetate through two-step coupling reaction | |
| CN114349598B (en) | Method for preparing 3-methylene-1, 5-pentanediol and 3-methyl-2-pentene-1, 5-diol | |
| CN111517927B (en) | Continuous preparation method of chloropropionaldehyde diol acetal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20071226 Termination date: 20120221 |