CN100369901C - Method for preparing 5,5-dimethylhydantion - Google Patents
Method for preparing 5,5-dimethylhydantion Download PDFInfo
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- CN100369901C CN100369901C CNB2006100380400A CN200610038040A CN100369901C CN 100369901 C CN100369901 C CN 100369901C CN B2006100380400 A CNB2006100380400 A CN B2006100380400A CN 200610038040 A CN200610038040 A CN 200610038040A CN 100369901 C CN100369901 C CN 100369901C
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- acetone cyanohydrin
- gas
- production method
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- ammoniacal liquor
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Abstract
The present invention discloses a preparation method of 5, 5-dimethylhydantoin, which comprises the steps that ammonia and acetone cyanohydrin are added to a reaction vessel and react; during reaction, the gas input valve of the reaction vessel and a gas output valve on a condenser connected with the reaction vessel are opened; ammonium carbonate converted gas is led in the reaction vessel until no cyanide group in reactant. The present invention fully utilizes CO2 in the converted gas, reduces the cost of a decarburizing device, reduces CO2 waste, performs a certain protective function to environments, increases the yield of liquid ammonia and increases economic benefit.
Description
Technical field:
The present invention relates to a kind of production method of 5,5 dimethyl hydantion.
Background technology:
Traditional dimethyl hydantion production technique, in 15% ammoniacal liquor, ammonia in molar ratio: acetone cyanohydrin=1: 0.9, drip acetone cyanohydrin at 10 ℃, 1/3 of adding ammonia molar weight bicarbonate of ammonia heats up and kept 20 minutes at 60 ℃ after adding, and adds the same bicarbonate of ammonia of measuring again and keeps 20 minutes, add same amount bicarbonate of ammonia at last and kept 20 minutes, the cooling blowing filters.Such technology utilization bicarbonate of ammonia adds thermogenesis CO
2, to waste ammonia wherein, and needed to open the reaction kettle cover in the operation, a large amount of ammonias come out.Cause environment abominable.
Summary of the invention:
The object of the present invention is to provide the environmental pollution of a kind of energy little, the production method of 5,5 dimethyl hydantion that production cost is low.
Technical solution of the present invention is:
A kind of 5, the production method of 5 dimethyl hydantion, it is characterized in that: comprise the following steps: in reactor, to add ammoniacal liquor, acetone cyanohydrin reacts, during reaction, open the gas input valve of reactor, and the gas delivery valve on unlatching and the condenser that reactor is connected, in reactor, feed carbon ammonium conversion gas, no cyanogen root to the reactant.
The mol ratio of ammoniacal liquor and acetone cyanohydrin is an ammoniacal liquor in the reaction raw materials: acetone cyanohydrin=1: 0.8.Acetone cyanohydrin is added drop-wise in the ammoniacal liquor under 30～40 ℃.Temperature of reaction is 60～70 ℃.The feeding speed of conversion gas is 3M
3/ minute.
The present invention makes full use of the CO in the conversion gas
2, reduced the cost of decarbonization device, reduced CO
2Waste, environment is played the certain protection effect, increased liquefied ammonia output, increased economic benefit.
The invention will be further described below in conjunction with embodiment.
Embodiment:
A kind of 5, the production method of 5 dimethyl hydantion, in reactor, add ammoniacal liquor, acetone cyanohydrin reacts, the mol ratio of ammoniacal liquor and acetone cyanohydrin is an ammoniacal liquor in the reaction raw materials: acetone cyanohydrin=1: 0.8, and acetone cyanohydrin is added drop-wise in the ammoniacal liquor under 30～40 ℃, add acetone cyanohydrin after, open the gas input valve of reactor, and the gas delivery valve on unlatching and the condenser that reactor is connected, (main component of conversion gas is: CO to feed carbon ammonium conversion gas in reactor
227%, H
255%, N
216%, CO 2%), the feeding speed of conversion gas is 3M
3/ minute, control reaction temperature is 60～70 ℃, flow quantity recorder feeds the total amount of conversion gas, feeds CO in the conversion gas
2After amount reached the molar weight of ammonia, whether sample examination had the cyanogen root, if any, continuing to feed conversion gas to check does not have the cyanogen root, after reaction finishes, closes and feeds valve, delivery valve, and the cooling blowing filters.The content that reaction finishes back conversion gas is CO
22%, H
273%, N
222%, CO3% send the carbon ammonium behind the refining post, makes liquefied ammonia.
Claims (5)
1. one kind 5, the production method of 5 dimethyl hydantion, it is characterized in that: comprise the following steps: in reactor, to add ammoniacal liquor, acetone cyanohydrin reacts, during reaction, open the gas input valve of reactor, and the gas delivery valve on unlatching and the condenser that reactor is connected, in reactor, feed carbon ammonium conversion gas, no cyanogen root to the reactant.
2. the production method of 5,5 dimethyl hydantion according to claim 1 is characterized in that: the mol ratio of ammoniacal liquor and acetone cyanohydrin is an ammoniacal liquor in the reaction raw materials: acetone cyanohydrin=1: 0.8.
3. the production method of 5,5 dimethyl hydantion according to claim 1 is characterized in that: acetone cyanohydrin is added drop-wise in the ammoniacal liquor under 30～40 ℃.
4. according to the production method of claim 1,2 or 3 described 5,5 dimethyl hydantion, it is characterized in that: temperature of reaction is 60～70 ℃.
5. according to the production method of claim 1,2 or 3 described 5,5 dimethyl hydantion, it is characterized in that: the feeding speed of conversion gas is 3M
3/ minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100380400A CN100369901C (en) | 2006-01-23 | 2006-01-23 | Method for preparing 5,5-dimethylhydantion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100380400A CN100369901C (en) | 2006-01-23 | 2006-01-23 | Method for preparing 5,5-dimethylhydantion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1803775A CN1803775A (en) | 2006-07-19 |
| CN100369901C true CN100369901C (en) | 2008-02-20 |
Family
ID=36865951
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100380400A Active CN100369901C (en) | 2006-01-23 | 2006-01-23 | Method for preparing 5,5-dimethylhydantion |
Country Status (1)
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| CN (1) | CN100369901C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002000B (en) * | 2010-11-18 | 2012-07-25 | 祝莉宁 | Method for producing 5,5-dimethyl hydantoin |
| CN102030712B (en) * | 2010-11-18 | 2012-02-01 | 大庆井井源油田科技开发有限公司 | Device for producing dimethyl hydantoin |
| CN108148000B (en) * | 2018-03-20 | 2020-03-27 | 河北利仕化学科技有限公司 | Preparation method of 5, 5-dimethylhydantoin |
| CN115703744A (en) * | 2021-11-16 | 2023-02-17 | 吉林市吉化江城油脂化工有限责任公司 | Preparation method of 5,5-dimethylhydantoin |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3752821A (en) * | 1967-08-18 | 1973-08-14 | Rheinpreussen Ag | Method for the continuous manufacture of hydantoins especially 5,5-dimethylhydantoin |
| EP0001394A2 (en) * | 1977-10-03 | 1979-04-18 | Lentia Gesellschaft mit beschränkter Haftung | Method for the continuous preparation of hydantoin derivatives, and apparatus for the application thereof |
| CN1235160A (en) * | 1999-04-20 | 1999-11-17 | 南京化工大学 | Preparation of 2,4-imidzolidinedione |
| CN1511831A (en) * | 2002-12-31 | 2004-07-14 | 中国人民解放军军事医学科学院放射医 | Process for preparing hydantoin |
| CN1616435A (en) * | 2004-09-15 | 2005-05-18 | 南京工业大学 | Process for preparing hydantoin by one-step method |
-
2006
- 2006-01-23 CN CNB2006100380400A patent/CN100369901C/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3752821A (en) * | 1967-08-18 | 1973-08-14 | Rheinpreussen Ag | Method for the continuous manufacture of hydantoins especially 5,5-dimethylhydantoin |
| EP0001394A2 (en) * | 1977-10-03 | 1979-04-18 | Lentia Gesellschaft mit beschränkter Haftung | Method for the continuous preparation of hydantoin derivatives, and apparatus for the application thereof |
| CN1235160A (en) * | 1999-04-20 | 1999-11-17 | 南京化工大学 | Preparation of 2,4-imidzolidinedione |
| CN1511831A (en) * | 2002-12-31 | 2004-07-14 | 中国人民解放军军事医学科学院放射医 | Process for preparing hydantoin |
| CN1616435A (en) * | 2004-09-15 | 2005-05-18 | 南京工业大学 | Process for preparing hydantoin by one-step method |
Non-Patent Citations (1)
| Title |
|---|
| 5，5-二甲基海因的合成. 徐章煌，李焰，黄锦霞，邹祖德.精细化工，第11卷第6期. 1994 * |
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|---|---|
| CN1803775A (en) | 2006-07-19 |
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Address after: 226407 Rudong Economic Development Zone, Nantong, the Yellow Sea, No., No. three road, No. 12 Patentee after: Jiangsu BICON Pharmaceutical Co., Ltd. Address before: 226401 Jiangsu Matang Town County of Rudong province Jianshe Road No. 40 Patentee before: Jiangsu Jiujiujiu Technology Co., Ltd. |
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Effective date of registration: 20171227 Address after: 226407 Rudong Economic Development Zone, Nantong, the Yellow Sea, No., No. three road, No. 12 Patentee after: Jiangsu nine Jiangsu jiujiujiu Technology Co. Ltd. Address before: 226407 Rudong Economic Development Zone, Nantong, the Yellow Sea, No., No. three road, No. 12 Patentee before: Jiangsu BICON Pharmaceutical Co., Ltd. |
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