CN101857534A - Technique for synthesizing methylal - Google Patents
Technique for synthesizing methylal Download PDFInfo
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- CN101857534A CN101857534A CN201010190078A CN201010190078A CN101857534A CN 101857534 A CN101857534 A CN 101857534A CN 201010190078 A CN201010190078 A CN 201010190078A CN 201010190078 A CN201010190078 A CN 201010190078A CN 101857534 A CN101857534 A CN 101857534A
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Abstract
The invention relates to a technique for synthesizing methylal, in particular to a technique for synthesizing methylal, which utilizes a reactive rectifying tower as a reaction container. The technique for synthesizing methylal carries out the reaction for synthesizing methylal in the reactive rectifying tower, methanol steam and formaldehyde solution enter the reactive rectifying tower respectively from the lower and the upper parts of the reactive rectifying tower, catalyst is placed on a tower plate of the reactive rectifying tower, the formaldehyde solution and the methanol steam react in the reactive rectifying tower to produce the methylal, the mixed steam of the methylal and the methanol enter a distillation tower and fractionated, the fractionated methanol solution flows back to the lower layer of the reactive rectifying tower and is heated for recycling, and after entering a condenser, the fractionated methylal is then condensed, so that finished methylal product is obtained. During reaction, the methanol is gaseous, consequently, the production of the mixture of the methylal and the methanol can be effectively reduced, and the purity of the finished methylal product can be increased. The unreacted methanol solution is distilled for recovery, consequently, the material utilization rate is increased, and the content of the methanol in wastewater is reduced.
Description
Technical field:
What the present invention relates to is a kind of technique for synthesizing methylal, especially a kind of technique for synthesizing methylal of utilizing reaction fractionating tower for reaction vessel.
Background technology:
The technology of traditional production methylal, employing is under sulphuric acid catalysis, methanol solution and formaldehyde solution are reacted in synthetic tower, because methyl alcohol is liquid during reaction, resultant of reaction methylal and methyl alcohol generate solution altogether easily, solution is difficult for separating from methylal altogether, thereby influences the quality of product methylal.Unreacted methanol solution is directly discharged, and causes in the waste of material and the waste water methanol content too high, contaminate environment.
Summary of the invention:
The objective of the invention is to provide a kind of growing amount that can effectively reduce methylal and methyl alcohol, improve the purity of product methylal.Improve utilization of materials, reduce the technique for synthesizing methylal of waste water methanol content.
Technical scheme of the present invention is
A kind of technique for synthesizing methylal, the reaction of synthesizing dimethoxym ethane is to carry out in reaction fractionating tower, methanol steam and formaldehyde solution enter reaction fractionating tower from the lower curtate and the top of reaction fractionating tower respectively, catalyzer is placed on the column plate, formaldehyde solution and methanol steam generate methylal at the reaction fractionating tower internal reaction, the mixing steam of methylal and methyl alcohol enters distillation tower and carries out fractionation, control distillation tower tower top temperature is at 42 ℃, the methanol solution that fractionates out is back to the reaction fractionating tower low layer and uses through heating cycle, and the methylal that fractionates out enters behind the condenser and promptly gets the methylal finished product after the condensation.
Preferably, the ratio of the amount of substance of methyl alcohol and formaldehyde is 2.1: 1～2.3: 1
Preferably, the temperature of reaction fractionating tower low layer is 95 ℃, and the temperature in the reaction fractionating tower is successively successively decreased from the bottom up, and the temperature of reaction fractionating tower top layer is 50 ℃.
Preferably, catalyzer is a storng-acid cation exchange resin.
Preferably, the weight of catalyzer is the 10%-20% of reaction mass weight.
The invention has the beneficial effects as follows: methyl alcohol is gaseous state during reaction, can effectively reduce methylal and the methyl alcohol growing amount of solution altogether, improves the purity of product methylal.Unreacted methanol solution reclaims through distillation, has improved utilization of materials, reduces the waste water methanol content.
Embodiment
A kind of technique for synthesizing methylal, the reaction of synthesizing dimethoxym ethane is to carry out in reaction fractionating tower, methanol steam and formaldehyde solution enter reaction fractionating tower from the low layer and the top layer of reaction fractionating tower respectively, wherein the proportional quantity of methyl alcohol and formaldehyde is 2.1: 1～2.3: 1, storng-acid cation exchange resin is placed on the column plate, formaldehyde solution and methanol steam generate methylal at the reaction fractionating tower internal reaction, during reaction, the temperature of reaction fractionating tower low layer is 95 ℃, temperature in the reaction fractionating tower is successively successively decreased from the bottom up, and the temperature of reaction fractionating tower top layer is 50 ℃.
The mixing steam of methylal and methyl alcohol enters distillation tower and carries out fractionation, and the methanol solution that fractionates out is back to the reaction fractionating tower low layer and recycles, and the methylal that fractionates out enters behind the condenser and promptly gets the methylal finished product after the condensation.
After reaction finishes the methanol solution of reaction fractionating tower bottom entered in the distiller and distill once more, the methanol steam condensation that distills out is recycled.
Claims (5)
1. technique for synthesizing methylal, it is characterized in that: the reaction of synthesizing dimethoxym ethane is to carry out in reaction fractionating tower, methanol steam and formaldehyde solution enter reaction fractionating tower from the low layer and the top layer of reaction fractionating tower respectively, be placed with catalyzer on the reaction fractionating tower column plate, formaldehyde solution and methanol steam generate methylal at the reaction fractionating tower internal reaction, the mixing steam of methylal and methyl alcohol enters distillation tower and carries out fractionation, control distillation tower tower top temperature is at 42 ℃, the methanol solution that fractionates out is back to the reaction fractionating tower low layer and uses through heating cycle, and the methylal that fractionates out enters behind the condenser and promptly gets the methylal finished product after the condensation.
2. according to the described a kind of technique for synthesizing methylal of claim 1, it is characterized in that: the ratio of the amount of substance of methyl alcohol and formaldehyde is 2.1: 1～2.3: 1.
3. according to the described a kind of technique for synthesizing methylal of claim 1, it is characterized in that: the temperature of reaction fractionating tower low layer is 95 ℃, and the temperature in the reaction fractionating tower is successively successively decreased from the bottom up, and the temperature of reaction fractionating tower top layer is 50 ℃.
4. according to the described a kind of technique for synthesizing methylal of claim 1, it is characterized in that: catalyzer is a storng-acid cation exchange resin.
5. according to the described a kind of technique for synthesizing methylal of claim 1, it is characterized in that: the weight of catalyzer is the 10%-20% of reaction mass weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010190078A CN101857534A (en) | 2010-06-03 | 2010-06-03 | Technique for synthesizing methylal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010190078A CN101857534A (en) | 2010-06-03 | 2010-06-03 | Technique for synthesizing methylal |
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| Publication Number | Publication Date |
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| CN101857534A true CN101857534A (en) | 2010-10-13 |
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| CN201010190078A Pending CN101857534A (en) | 2010-06-03 | 2010-06-03 | Technique for synthesizing methylal |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351665A (en) * | 2011-08-17 | 2012-02-15 | 中国科学院新疆理化技术研究所 | Preparation method of methylal |
| CN103664551A (en) * | 2013-12-03 | 2014-03-26 | 惠州市利而安化工有限公司 | Synthesis method of methylal |
| JP2014507371A (en) * | 2010-11-09 | 2014-03-27 | イオネス パラフォルム ゲーエムベーハー ウント コムパニー カーゲー | How to make pure 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 |
| 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 |
| CN105669454A (en) * | 2014-11-17 | 2016-06-15 | 中国科学院大连化学物理研究所 | Method for preparing methyl formate |
| CN109574981A (en) * | 2019-01-15 | 2019-04-05 | 浙江昊唐实业有限公司 | A method of preparing glycerin shrinkage benzaldehyde |
| CN111807940A (en) * | 2020-07-21 | 2020-10-23 | 安徽金轩科技有限公司 | Method for recycling waste methanol in galaxolide production |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0570719A1 (en) * | 1992-04-24 | 1993-11-24 | Showa Denko Kabushiki Kaisha | Process for producing acetaldehyde dimethylacetal |
| CN1160392A (en) * | 1994-10-07 | 1997-09-24 | 旭化成工业株式会社 | Method of refining methylal |
| CN1807378A (en) * | 2006-01-26 | 2006-07-26 | 南京师范大学 | Method for preparing methylal using combined continuous distillation and liquid-liquid extraction |
| CN101094825A (en) * | 2004-12-09 | 2007-12-26 | 泰科纳有限公司 | Method for the production of acetals |
-
2010
- 2010-06-03 CN CN201010190078A patent/CN101857534A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0570719A1 (en) * | 1992-04-24 | 1993-11-24 | Showa Denko Kabushiki Kaisha | Process for producing acetaldehyde dimethylacetal |
| CN1160392A (en) * | 1994-10-07 | 1997-09-24 | 旭化成工业株式会社 | Method of refining methylal |
| CN101094825A (en) * | 2004-12-09 | 2007-12-26 | 泰科纳有限公司 | Method for the production of acetals |
| CN1807378A (en) * | 2006-01-26 | 2006-07-26 | 南京师范大学 | Method for preparing methylal using combined continuous distillation and liquid-liquid extraction |
Non-Patent Citations (2)
| Title |
|---|
| 周伟等: "催化精馏在合成甲缩醛中的应用", 《工业催化》, no. 1, 15 February 1998 (1998-02-15), pages 35 - 39 * |
| 秦娟妮等: "甲缩醛反应精馏过程模拟", 《当代化工》, vol. 36, no. 3, 28 June 2007 (2007-06-28), pages 285 - 287 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014507371A (en) * | 2010-11-09 | 2014-03-27 | イオネス パラフォルム ゲーエムベーハー ウント コムパニー カーゲー | How to make pure methylal |
| CN102351665A (en) * | 2011-08-17 | 2012-02-15 | 中国科学院新疆理化技术研究所 | Preparation method of methylal |
| CN103664551A (en) * | 2013-12-03 | 2014-03-26 | 惠州市利而安化工有限公司 | Synthesis method of 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 |
| 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 |
| CN105669454A (en) * | 2014-11-17 | 2016-06-15 | 中国科学院大连化学物理研究所 | Method for preparing methyl formate |
| CN109574981A (en) * | 2019-01-15 | 2019-04-05 | 浙江昊唐实业有限公司 | A method of preparing glycerin shrinkage benzaldehyde |
| CN109574981B (en) * | 2019-01-15 | 2020-06-23 | 上海芜玮环境科技有限公司 | Method for preparing glycerol benzaldehyde |
| CN111807940A (en) * | 2020-07-21 | 2020-10-23 | 安徽金轩科技有限公司 | Method for recycling waste methanol in galaxolide production |
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Application publication date: 20101013 |