CN1911901A - Production technology of formamide - Google Patents

Production technology of formamide Download PDF

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Publication number
CN1911901A
CN1911901A CN 200610068436 CN200610068436A CN1911901A CN 1911901 A CN1911901 A CN 1911901A CN 200610068436 CN200610068436 CN 200610068436 CN 200610068436 A CN200610068436 A CN 200610068436A CN 1911901 A CN1911901 A CN 1911901A
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CN
China
Prior art keywords
product
methane amide
tower
methyl
formiate
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Pending
Application number
CN 200610068436
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Chinese (zh)
Inventor
张炳胜
陈衍军
周树新
徐衍桥
武峰
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张炳胜
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Publication date
Application filed by 张炳胜 filed Critical 张炳胜
Priority to CN 200610068436 priority Critical patent/CN1911901A/en
Publication of CN1911901A publication Critical patent/CN1911901A/en
Pending legal-status Critical Current

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Abstract

The formamide producing process belongs to the field of chemical product producing technology. The technological scheme includes the following steps: the combination reaction of methyl formate and ammonia in a tank reactor and storing the reacted liquid in a storage tank; the subsequent pumping reacted liquid into crude distillation column for distillation dealcholizing while recovering un-reacted methyl formate and ammonia and side product methanol; the vacuum rectification of the crude product in a dealcholizing tower to eliminate small amount of methanol of formamide product; refining of the tower bottom material in a refining tower to eliminate micro amount of low boiling point matters; and adsorbing with cocoanut active carbon in an adsorbing tower to eliminate micro amount of high boiling point matter and to obtain formamide product. The process has low production cost.

Description

A kind of production technology of formamide
Technical field: the present invention relates to the Chemicals technical field of producing, is a kind of production technology of formamide more specifically.
Background technology: domestic early stage several families methane amide dingus adopts ethyl formate and ammonia synthesis technology, and this is backward in technique, and quality product is low, now to the edge that is eliminated.Have only manufacturer of 2-3 family to adopt methanol dehydrogenation system methyl-formiate, methane amide technology is produced in ammonification again, production cost is higher, has limited at home widely-used of methane amide product.
Summary of the invention:, the objective of the invention is to invent a kind of production technology of formamide for overcoming above-mentioned shortcoming.Its technical scheme is: will carry out building-up reactions in methyl-formiate and the ammonia input tank reactor under normal pressure, 40-50 ℃ temperature, reactant enters the reaction solution basin; Then reactant is distilled dealcoholysis with pump input topping still, this moment, distillation tower pressure was-0.07MPA tower top temperature 20-30 ℃, column bottom temperature 90-115 ℃, reclaim unreacted methyl-formiate and ammonia, reclaim byproduct methyl alcohol simultaneously, by-product methyl alcohol is sent the methyl-formiate production equipment back to as raw material; Thick product enters dealcoholize column and carries out rectification under vacuum, removes the small amount of methanol in the methane amide; The bottoms material enters the treating tower of vacuum tightness-0.095--0.097MPA again and makes with extra care, and further removes the micro-low boilers in the methane amide; The methane amide product enters adsorption tower absorption, under the effect of cocoanut active charcoal sorbent material, removes micro-high boiling substance and makes the methane amide product.The advantage of this invention is: the more domestic existing processes of methane amide production cost that makes by this production technique reduces greatly, amination process using domestic first cover high vacuum rectification technology and efficient adsorption technology, do not add any catalyzer, reaction simultaneously is operate continuously, the state of the art place is leading domestic, price advantage is obvious, this project implementation can change the situation of China's high-quality methane amide product dependence on import, can create and save a large amount of foreign exchanges for country, economic and social benefit is remarkable, has promoted the large-scale application of domestic methane amide product at medicine, pesticide industry; Behind the launch products, be subjected to domestic and international client's consistent favorable comment.
Embodiment:
One, produces the example of 1 ton of methane amide
1,1360Kg methyl-formiate and 378Kg ammonia are entered in the tank reactor after metering (the excessive 1-2% of methyl-formiate) carry out building-up reactions under normal pressure, 40 ℃ of temperature, reactant enters the reaction solution basin;
2, then reactant is distilled dealcoholysis with pump input topping still, this moment, distillation tower pressure was-0.07MPA 20 ℃ of tower top temperatures, 90 ℃ of column bottom temperatures, reclaim unreacted methyl-formiate and ammonia, reclaim byproduct methyl alcohol simultaneously, by-product methyl alcohol is sent the methyl-formiate production equipment back to as raw material;
3, thick product enters dealcoholize column and carries out rectification under vacuum, removes the low-boiling point materials such as small amount of methanol in the methane amide;
4, the bottoms material treating tower that enters vacuum tightness-0.095MPA is again made with extra care, and further removes the micro-low boilers in the methane amide;
5, the methane amide product enters adsorption tower absorption, under the effect of cocoanut active charcoal sorbent material, removes the micro-high boiling substance that is generated when fluctuating because of operational condition, to reach the requirement of product to colourity, obtains the methane amide product of 1000Kg;
6, be packaged into the product methane amide at last.
Two, produce the example of 500Kg methane amide:
1,680Kg methyl-formiate and 189Kg ammonia are entered in the tank reactor after metering (the excessive 1-2% of methyl-formiate) carry out building-up reactions under normal pressure, 45 ℃ of temperature, reactant enters the reaction solution basin;
2, then reactant is distilled dealcoholysis with pump input topping still, this moment, distillation tower pressure was-0.07MPA 25 ℃ of tower top temperatures, 102.5 ℃ of column bottom temperatures, reclaim unreacted methyl-formiate and ammonia, reclaim byproduct methyl alcohol simultaneously, by-product methyl alcohol is sent the methyl-formiate production equipment back to as raw material;
3, thick product enters dealcoholize column and carries out rectification under vacuum, removes the low-boiling point materials such as small amount of methanol in the methane amide;
4, the bottoms material treating tower that enters vacuum tightness-0.096MPA is again made with extra care, and further removes the micro-low boilers in the methane amide;
5, the methane amide product enters adsorption tower absorption, under the effect of cocoanut active charcoal sorbent material, removes the micro-high boiling substance that is generated when fluctuating because of operational condition, to reach the requirement of product to colourity, obtains the methane amide product of 500Kg;
6, be packaged into the product methane amide at last.
Three, produce the example of 250Kg methane amide:
1,340Kg methyl-formiate and 94.5Kg ammonia are entered in the tank reactor after metering (the excessive 1-2% of methyl-formiate) carry out building-up reactions under normal pressure, 50C temperature, reactant enters the reaction solution basin;
2, then reactant is distilled dealcoholysis with pump input topping still, this moment, distillation tower pressure was-0.07MPA 30 ℃ of tower top temperatures, 115 ℃ of column bottom temperatures, reclaim unreacted methyl-formiate and ammonia, reclaim byproduct methyl alcohol simultaneously, by-product methyl alcohol is sent the methyl-formiate production equipment back to as raw material;
3, thick product enters dealcoholize column and carries out rectification under vacuum, removes the low-boiling point materials such as small amount of methanol in the methane amide;
4, the bottoms material treating tower that enters vacuum tightness-0.097MPA is again made with extra care, and further removes the micro-low boilers in the methane amide;
5, the methane amide product enters adsorption tower absorption, under the effect of cocoanut active charcoal sorbent material, removes the micro-high boiling substance that is generated when fluctuating because of operational condition, to reach the requirement of product to colourity, obtains the methane amide product of 250Kg;
6, be packaged into the product methane amide at last.

Claims (1)

1, a kind of production technology of formamide is characterized in that: will carry out building-up reactions in methyl-formiate and the ammonia input tank reactor under normal pressure, 40-50 ℃ temperature, reactant enters the reaction solution basin; Then reactant is distilled dealcoholysis with pump input topping still, this moment, distillation tower pressure was-0.07MPA tower top temperature 20-30 ℃, column bottom temperature 90-115 ℃, reclaim unreacted methyl-formiate and ammonia, reclaim byproduct methyl alcohol simultaneously, by-product methyl alcohol is sent the methyl-formiate production equipment back to as raw material; Thick product enters dealcoholize column and carries out rectification under vacuum, removes the small amount of methanol in the methane amide; The bottoms material enters the treating tower of vacuum tightness-0.095--0.097MPA again and makes with extra care, and further removes the micro-low boilers in the methane amide; The methane amide product enters adsorption tower absorption, under the effect of cocoanut active charcoal sorbent material, removes micro-high boiling substance and makes the methane amide product.
CN 200610068436 2006-08-25 2006-08-25 Production technology of formamide Pending CN1911901A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200610068436 CN1911901A (en) 2006-08-25 2006-08-25 Production technology of formamide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200610068436 CN1911901A (en) 2006-08-25 2006-08-25 Production technology of formamide

Publications (1)

Publication Number Publication Date
CN1911901A true CN1911901A (en) 2007-02-14

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN 200610068436 Pending CN1911901A (en) 2006-08-25 2006-08-25 Production technology of formamide

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CN (1) CN1911901A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109336822A (en) * 2018-11-27 2019-02-15 湖北省宏源药业科技股份有限公司 A kind of metronidazole production method
CN109761841A (en) * 2019-01-30 2019-05-17 上海阿拉丁生化科技股份有限公司 A kind of preparation process of order of spectrum formamide
CN111606821A (en) * 2020-06-03 2020-09-01 江苏巨莱生物医药有限公司 Formamide purification process
CN114853570A (en) * 2022-05-13 2022-08-05 山东阿斯德科技有限公司 Method for treating wastewater in formamide production device

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109336822A (en) * 2018-11-27 2019-02-15 湖北省宏源药业科技股份有限公司 A kind of metronidazole production method
CN109761841A (en) * 2019-01-30 2019-05-17 上海阿拉丁生化科技股份有限公司 A kind of preparation process of order of spectrum formamide
CN111606821A (en) * 2020-06-03 2020-09-01 江苏巨莱生物医药有限公司 Formamide purification process
CN111606821B (en) * 2020-06-03 2023-08-11 江苏巨莱生物医药有限公司 Purification process of formamide
CN114853570A (en) * 2022-05-13 2022-08-05 山东阿斯德科技有限公司 Method for treating wastewater in formamide production device

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