CN1304369C - Technique for preparing dimehtyl sulfate - Google Patents
Technique for preparing dimehtyl sulfate Download PDFInfo
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- CN1304369C CN1304369C CNB2004101553338A CN200410155333A CN1304369C CN 1304369 C CN1304369 C CN 1304369C CN B2004101553338 A CNB2004101553338 A CN B2004101553338A CN 200410155333 A CN200410155333 A CN 200410155333A CN 1304369 C CN1304369 C CN 1304369C
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- sulfate
- dimethyl ether
- methyl
- gas
- preparation technology
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- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The present invention provides an improved production process for dimethyl sulfate. After etherification reaction, two-stage condensation is changed into an alkali treatment process, i.e. dimethyl ether gas obtained in the etherification reaction is firstly led in an alkali liquor absorption tank for neutralization reaction so as to remove acid; the gas subsequently enters a methanol recovery device, and water and methanol are removed for esterification reaction. The improved production process solves the problem of production device corrosion because of the acid in the dimethyl ether gas, and the neutralized dimethyl ether gas can also be used for methanol recovery, so the quality of the dimethyl ether gas is improved, and the product quality of final dimethyl sulfate is further increased.
Description
Technical field
The present invention relates to the preparation technology of Organic Chemicals methyl-sulfate.
Background technology
Methyl-sulfate is a methylating agent good in the organic synthesis, is widely used in the industry such as chemical industry, medicine, agricultural chemicals, rubber and leather, and be a kind of important chemical material.
Production Flow Chart at present is roughly:
1, joins catalyst: sulfuric acid+methyl alcohol → methyl-hydrogen-sulfate monomethyl-sulfate
2, etherificate: methyl-hydrogen-sulfate monomethyl-sulfate+methyl alcohol → dme
3, esterification: dme+sulphur trioxide → methyl-sulfate
Because in the second step etherification procedure, temperature of reaction is higher, the gas of dimethyl ether that generates can be taken water and acid out of, former process using condensed in two stages mode dewaters and acid, but because the deacidification effect is not thorough, always contain certain acid in the methyl ether gas, therefore, influence the industrialization continuous production producing certain corrosion to production unit in the suitability for industrialized production for a long time.
Summary of the invention
The present invention is for solving the problem that above-mentioned technology exists, original production process is improved, behind etherification reaction, change condensed in two stages into alkaline purification, solved and contained acid in the gas of dimethyl ether for a long time to production unit corrosive problem, and the gas of dimethyl ether after the neutralization can also carry out the Methanol Recovery utilization, the quality of gas of dimethyl ether is improved, and then improved the quality product of final methyl-sulfate.
The preparation technology of methyl-sulfate of the present invention generates methyl-hydrogen-sulfate monomethyl-sulfate with sulfuric acid and methyl alcohol, generates methyl-sulfate through etherificate, esterification again, it is characterized in that dme behind the etherification reaction is by alkaline purification after, carry out esterification again.
Former technical process:
Sulfuric acid+methyl alcohol → etherificate → one-level condensation → B-grade condensation → dme → esterification
Existing technical process:
Sulfuric acid+methyl alcohol → etherificate → alkaline purification → reclaim respectively first alcohol and water → dme → esterification
The present invention changes condensed in two stages into alkali pretreatment behind etherification reaction.
Described alkali pretreatment is that the gas of dimethyl ether that etherificate obtains at first feeds the alkali lye tourie, carries out neutralization reaction, removes disacidify, and then enters Methanol Recovery equipment (common water alcohol separating device), adds heat extraction water and methyl alcohol, carries out esterification again.
Wherein used concentration of lye scope is 8%----38% (weight percentage), and preferable range is 20%-----23% (weight percentage).Alkali lye preferably adopts liquid caustic soda.
The invention solves in the production process because of containing acid in the gas of dimethyl ether for a long time to production unit corrosive problem, and the gas of dimethyl ether after the neutralization can also carry out the Methanol Recovery utilization, the quality of gas of dimethyl ether is improved, and then improved the quality product of final methyl-sulfate.
Embodiment:
In the etherification reaction operation, logical methyl alcohol 1390kg in methyl-hydrogen-sulfate monomethyl-sulfate, 140～150 ℃ of control reaction temperature, the gas of dimethyl ether of generation removes disacidify through the liquid caustic soda tourie earlier, gets qualified methyl alcohol 216kg through fractionation again, gas of dimethyl ether is fed the esterification jar again.
Have the sulphur trioxide of absorption in the esterification jar, control under 90～100 ℃ of conditions, with the gas of dimethyl ether reaction that feeds, after about 3 hours, get methyl-sulfate crude product 2200kg, underpressure distillation under vacuum tightness 0.09Mpa condition again, get finished product methyl-sulfate 2090kg, yield 90.37%, content 98.60%, acidity 0.45%.
The same operation, according to the concentration difference of alkaline purification alkali lye, handle dme respectively after, carry out esterification, the result is as follows:
| Alkali concn W/W | 8％ | 15％ | 20％ | 23％ | 38％ |
| Former pH value | 6.0 | 6.0 | 5.0 | 5.0 | 5.0 |
| Existing pH value | 7.0 | 7.0 | 7.0 | 7.0 | 7.0 |
After alkaline purification, esterification yield and product yield are unaffected.
Claims (5)
1. the preparation technology of a methyl-sulfate generates methyl-hydrogen-sulfate monomethyl-sulfate with sulfuric acid and methyl alcohol, generates methyl-sulfate through etherificate, esterification again, it is characterized in that dme behind the etherification reaction is by alkaline purification after, carry out esterification again.
2. preparation technology according to claim 1 is characterized in that dme is through after the alkaline purification, again through Methanol Recovery.
3. preparation technology according to claim 1 and 2 is characterized in that, the concentration of lye scope that described alkaline purification is used percentage ratio is by weight counted 8%----38%.
4. preparation technology according to claim 1 and 2 is characterized in that, the concentration of lye scope that described alkaline purification is used percentage ratio is by weight counted 20%------23%.
5. preparation technology according to claim 1 and 2 is characterized in that the alkali that described alkaline purification is used is liquid caustic soda.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004101553338A CN1304369C (en) | 2004-10-12 | 2004-10-12 | Technique for preparing dimehtyl sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004101553338A CN1304369C (en) | 2004-10-12 | 2004-10-12 | Technique for preparing dimehtyl sulfate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1760179A CN1760179A (en) | 2006-04-19 |
| CN1304369C true CN1304369C (en) | 2007-03-14 |
Family
ID=36706425
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004101553338A Expired - Fee Related CN1304369C (en) | 2004-10-12 | 2004-10-12 | Technique for preparing dimehtyl sulfate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1304369C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249953A (en) * | 2011-05-20 | 2011-11-23 | 山东兴辉化工有限公司 | Method for converting dimethyl sulfate waste residue into dimethyl sulfate product |
| CN102659584A (en) * | 2012-05-21 | 2012-09-12 | 天津市碳一有机合成工程设计有限公司 | Chemical reaction system for producing oxalic acid diester as main products by using sodium formate as raw materials |
| CN104774162B (en) * | 2014-01-09 | 2017-02-08 | 泰安汉威化工有限公司 | Method used for preparing diethyl sulfate |
| CN105130850A (en) * | 2015-09-17 | 2015-12-09 | 湖北远大富驰医药化工股份有限公司 | Method for purifying dimethyl sulfate |
| CN115028555B (en) * | 2022-07-04 | 2023-09-29 | 武汉青江化工黄冈有限公司 | Continuous synthesis process of diethyl sulfate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86105064A (en) * | 1986-08-09 | 1987-04-22 | 山东新华制药厂 | The lower concentration sulphur trioxide is made the method for methyl-sulfate |
| CN1036199A (en) * | 1986-11-18 | 1989-10-11 | 莱茵河褐煤动力燃料联合有限公司 | Produce the method for pure Dimethyl ether |
| WO2001017937A1 (en) * | 1999-09-09 | 2001-03-15 | Siemens Axiva Gmbh & Co. Kg | Method for producing dimethylether |
-
2004
- 2004-10-12 CN CNB2004101553338A patent/CN1304369C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86105064A (en) * | 1986-08-09 | 1987-04-22 | 山东新华制药厂 | The lower concentration sulphur trioxide is made the method for methyl-sulfate |
| CN1036199A (en) * | 1986-11-18 | 1989-10-11 | 莱茵河褐煤动力燃料联合有限公司 | Produce the method for pure Dimethyl ether |
| WO2001017937A1 (en) * | 1999-09-09 | 2001-03-15 | Siemens Axiva Gmbh & Co. Kg | Method for producing dimethylether |
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| Publication number | Publication date |
|---|---|
| CN1760179A (en) | 2006-04-19 |
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Granted publication date: 20070314 Termination date: 20101012 |