CN1683324A - Novel process for cleanly producing acetamidine hydrochloride - Google Patents
Novel process for cleanly producing acetamidine hydrochloride Download PDFInfo
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- CN1683324A CN1683324A CN 200510037947 CN200510037947A CN1683324A CN 1683324 A CN1683324 A CN 1683324A CN 200510037947 CN200510037947 CN 200510037947 CN 200510037947 A CN200510037947 A CN 200510037947A CN 1683324 A CN1683324 A CN 1683324A
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- methyl alcohol
- synthetic
- ethanamidine
- inferior
- ammonification
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Abstract
The clean production process of acetamidine hydrochloride includes the following steps: synthesis of methanol hydrochloride, synthesis of ethylidene amidine, synthesis of aminomethanol, ammonation of ethylidene amidine, concentration and centrifugation. The present invention features that hydrogen chloride gas for the synthesis of methanol hydrochloride is side product of paraffin chloride producing process, and has simple technological process, low production cost, high product yield and no environmental pollution.
Description
Technical field
What the present invention relates to is a kind of acyclic or isocyclic compound, relates in particular to a kind of have nitrogen and carbon bonded or nitrogen and carbon and hydrogen bonded compound.
Background technology
The method of production acetamidine hydrochloride mainly adopts acid catalyzed process at present, traditional acid catalyzed process mainly is with chlorsulfonic acid and hydrochloric acid or sulfuric acid and the hydrochloric acid reaction generation hydrogen chloride gas raw material as sour methyl alcohol operation, produce a large amount of sulfur waste acid that contains 5-8% hydrogenchloride in the production process, be difficult to administer and utilize, the discontinuous cyclical operation of production technique, and hydrogen chloride gas absorbs under barotropic state, in the production process withstand voltage, requirement for anticorrosion is higher, very easily produce uncontrollable discharge, cause very big pollution to environment, increased production cost greatly; Simultaneously, this traditional technology off-set facility is various, and floor space is big, the energy consumption height, and raw material consumption height, product yield are low.
Summary of the invention
The purpose of this invention is to provide a kind of novel process for cleanly producing acetamidine hydrochloride, this technology has overcome the deficiency of traditional technology, and the high purity superchlorination hydrogen that utilizes by-product in the chlorinated-paraffin producing process process is as raw material, technology is simple, production cost is low, product yield height, non-pollutant discharge.
The present invention solves the problems of the technologies described above by following technical proposal to realize, above-mentioned novel process for cleanly producing acetamidine hydrochloride, and it comprises:
(1) sour methyl alcohol is synthetic: hydrogen chloride gas enters sour methyl alcohol Preparation tank through the graphite cooler cooling, synthetic sour methyl alcohol;
(2) inferior ethanamidine is synthetic: synthetic acid methyl alcohol is entered synthesis reactor and acetonitrile reaction, and acetonitrile drips by elevated dosing vessel, and about 4-5h dropwises, and insulation was lowered the temperature after a few hours, and methyl alcohol is added synthesis reactor, diluted inferior ethanamidine;
(3) ammonia methyl alcohol is synthetic: liquefied ammonia is flowed into Preparation tank, be dissolved in the methyl alcohol, the Preparation tank coil pipe feeds chilled brine, synthetic ammonia methyl alcohol;
(4) ammonification of inferior ethanamidine: synthetic ammonia methyl alcohol and inferior ethanamidine are entered ammonification in the ammonification still, and the ammonification temperature is controlled at 35-55 ℃, and the ph value should be about 7.5-9.0;
(5) concentrate and centrifugal: the material after the inferior ethanamidine ammonification advances whizzer isolate side product sodium chloride after, mother liquor is sent into rectification working process and is reclaimed methyl alcohol, reclaiming methyl alcohol returns into operation (3) synthetic ammonia methyl alcohol, the mother liquor that reclaims behind the methyl alcohol goes out the acetamidine hydrochloride product through concentrating under reduced pressure, cooling, centrifugation again, and the centrifugal secondary mother liquid that goes out is partly sneaked into down and criticized a mother liquor.
Difference is that the raw material hydrogen chloride gas in the above-mentioned sour methyl alcohol synthesis procedure is the by-product hydrogen chloride gas in the chlorinated-paraffin producing process process.
Raw material hydrogen chloride gas in the above-mentioned sour methyl alcohol synthesis procedure is adopting saturated solution of ferrous chloride convection current absorption impurity chlorine wherein after atomizing.
Above-mentioned sour methyl alcohol synthesis procedure adopts secondary the pressure to absorb.
The present invention compared with prior art has following advantage: above-mentioned novel process for cleanly producing acetamidine hydrochloride, the high purity superchlorination hydrogen that has utilized by-product in the chlorinated-paraffin producing process process is as raw material, reduced with chlorsulfonic acid and hydrochloric acid or sulfuric acid and hydrochloric acid reaction generation hydrogen chloride gas operation, adopt totally-enclosed systemic circulation operation simultaneously, technology is simple, production cost reduces 10-15%, and product yield improves 5-10%, does not have " three wastes " discharging in the production process.
Embodiment
Embodiment.
A kind of novel process for cleanly producing acetamidine hydrochloride, it comprises:
(1) sour methyl alcohol is synthetic: the by-product hydrogen chloride gas in the chlorinated-paraffin producing process process, adopt saturated solution of ferrous chloride convection current absorption impurity chlorine wherein after atomizing, enter sour methyl alcohol Preparation tank through the graphite cooler cooling again, adopt secondary the pressure to absorb, synthetic sour methyl alcohol;
(2) inferior ethanamidine is synthetic: synthetic acid methyl alcohol is entered synthesis reactor and acetonitrile reaction, and acetonitrile drips by elevated dosing vessel, and about 4-5h dropwises, and insulation was lowered the temperature after a few hours, and methyl alcohol is added synthesis reactor, diluted inferior ethanamidine;
(3) ammonia methyl alcohol is synthetic: liquefied ammonia is flowed into Preparation tank, be dissolved in the methyl alcohol, the Preparation tank coil pipe feeds chilled brine, synthetic ammonia methyl alcohol;
(4) ammonification of inferior ethanamidine: synthetic ammonia methyl alcohol and inferior ethanamidine are entered ammonification in the ammonification still, and the ammonification temperature is controlled at 35-55 ℃, and the ph value should be about 7.5-9.0;
(5) concentrate and centrifugal: the material after the inferior ethanamidine ammonification advances whizzer isolate side product sodium chloride after, mother liquor is sent into rectification working process and is reclaimed methyl alcohol, reclaiming methyl alcohol returns into operation (3) synthetic ammonia methyl alcohol, the mother liquor that reclaims behind the methyl alcohol goes out the acetamidine hydrochloride product through concentrating under reduced pressure, cooling, centrifugation again, and the centrifugal secondary mother liquid that goes out is partly sneaked into down and criticized a mother liquor.
Claims (3)
1, a kind of novel process for cleanly producing acetamidine hydrochloride, it comprises:
(1) sour methyl alcohol is synthetic: hydrogen chloride gas enters sour methyl alcohol Preparation tank through the graphite cooler cooling, synthetic sour methyl alcohol;
(2) inferior ethanamidine is synthetic: synthetic acid methyl alcohol is entered synthesis reactor and acetonitrile reaction, and acetonitrile drips by elevated dosing vessel, and about 4-5h dropwises, and insulation was lowered the temperature after a few hours, and methyl alcohol is added synthesis reactor, diluted inferior ethanamidine;
(3) ammonia methyl alcohol is synthetic: liquefied ammonia is flowed into Preparation tank, be dissolved in the methyl alcohol, the Preparation tank coil pipe feeds chilled brine, synthetic ammonia methyl alcohol;
(4) ammonification of inferior ethanamidine: synthetic ammonia methyl alcohol and inferior ethanamidine are entered ammonification in the ammonification still, and the ammonification temperature is controlled at 35-55 ℃, and the ph value should be about 7.5-9.0;
(5) concentrate and centrifugal: the material after the inferior ethanamidine ammonification advances whizzer isolate side product sodium chloride after, mother liquor is sent into rectification working process and is reclaimed methyl alcohol, reclaiming methyl alcohol returns into operation (3) synthetic ammonia methyl alcohol, the mother liquor that reclaims behind the methyl alcohol goes out the acetamidine hydrochloride product through concentrating under reduced pressure, cooling, centrifugation again, and the centrifugal secondary mother liquid that goes out is partly sneaked into down and criticized a mother liquor;
It is characterized in that: the raw material hydrogen chloride gas in the above-mentioned sour methyl alcohol synthesis procedure is the by-product hydrogen chloride gas in the chlorinated-paraffin producing process process.
2, novel process for cleanly producing acetamidine hydrochloride according to claim 1 is characterized in that: the raw material hydrogen chloride gas in the above-mentioned sour methyl alcohol synthesis procedure is adopting saturated solution of ferrous chloride convection current absorption impurity chlorine wherein after atomizing.
3, novel process for cleanly producing acetamidine hydrochloride according to claim 2 is characterized in that: above-mentioned sour methyl alcohol synthesis procedure adopts secondary the pressure to absorb.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510037947 CN1683324A (en) | 2005-03-02 | 2005-03-02 | Novel process for cleanly producing acetamidine hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510037947 CN1683324A (en) | 2005-03-02 | 2005-03-02 | Novel process for cleanly producing acetamidine hydrochloride |
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| CN1683324A true CN1683324A (en) | 2005-10-19 |
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| CN 200510037947 Pending CN1683324A (en) | 2005-03-02 | 2005-03-02 | Novel process for cleanly producing acetamidine hydrochloride |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134737B (en) * | 2006-08-30 | 2010-05-12 | 王志浩 | Process for synthesizing ethenylamidine hydrochloride by one-step method |
| CN107141194A (en) * | 2017-05-26 | 2017-09-08 | 湖北泰盛化工有限公司 | A kind of sour methanol of Joint Production, the equipment and technique of chloromethanes |
| CN110038459A (en) * | 2019-05-22 | 2019-07-23 | 蚌埠学院 | A kind of device and preparation method thereof preparing hydrogen chloride methanol solution |
| CN111269145A (en) * | 2020-03-11 | 2020-06-12 | 唐山威格化学工业有限公司 | Preparation method of acetamidine hydrochloride |
| CN112679387A (en) * | 2020-12-31 | 2021-04-20 | 江苏兄弟维生素有限公司 | Preparation method and application of acetamidine hydrochloride |
| CN113968800A (en) * | 2021-11-08 | 2022-01-25 | 内蒙古恒茂鑫精细化工有限公司 | Preparation method and device of acetamidine hydrochloride and use method of device |
-
2005
- 2005-03-02 CN CN 200510037947 patent/CN1683324A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134737B (en) * | 2006-08-30 | 2010-05-12 | 王志浩 | Process for synthesizing ethenylamidine hydrochloride by one-step method |
| CN107141194A (en) * | 2017-05-26 | 2017-09-08 | 湖北泰盛化工有限公司 | A kind of sour methanol of Joint Production, the equipment and technique of chloromethanes |
| CN107141194B (en) * | 2017-05-26 | 2023-07-28 | 湖北泰盛化工有限公司 | Equipment and process for jointly producing acid methanol and chloromethane |
| CN110038459A (en) * | 2019-05-22 | 2019-07-23 | 蚌埠学院 | A kind of device and preparation method thereof preparing hydrogen chloride methanol solution |
| CN110038459B (en) * | 2019-05-22 | 2024-01-19 | 蚌埠学院 | Device for preparing hydrogen chloride methanol solution and preparation method thereof |
| CN111269145A (en) * | 2020-03-11 | 2020-06-12 | 唐山威格化学工业有限公司 | Preparation method of acetamidine hydrochloride |
| CN112679387A (en) * | 2020-12-31 | 2021-04-20 | 江苏兄弟维生素有限公司 | Preparation method and application of acetamidine hydrochloride |
| CN112679387B (en) * | 2020-12-31 | 2023-01-03 | 江苏兄弟维生素有限公司 | Preparation method and application of acetamidine hydrochloride |
| CN113968800A (en) * | 2021-11-08 | 2022-01-25 | 内蒙古恒茂鑫精细化工有限公司 | Preparation method and device of acetamidine hydrochloride and use method of device |
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