CN100395229C - Process for low pressure synthesizing 3-pentylamine - Google Patents
Process for low pressure synthesizing 3-pentylamine Download PDFInfo
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- CN100395229C CN100395229C CNB200510018354XA CN200510018354A CN100395229C CN 100395229 C CN100395229 C CN 100395229C CN B200510018354X A CNB200510018354X A CN B200510018354XA CN 200510018354 A CN200510018354 A CN 200510018354A CN 100395229 C CN100395229 C CN 100395229C
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- synthetic
- synthesizing
- pentylamine
- preheating
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Abstract
The present invention relates to technology for synthesizing 3-pentylamine by a low pressure method. 3-pentanone, liquid ammonia and hydrogen gas are used as raw materials of synthesis, and Ni-Cr-HPO3 and Al2O3 are used as catalysts. The synthetic technology comprises: 3-pentanone, liquid ammonia and hydrogen gas are added into a preheating mixer according to the mole ratio of 0.5 to 2:1 to 5:2 to 7 to be preheated and mixed; then, the mixture enters a synthesizing tower with Ni-Cr-HPO3 and Al2O3 as catalysts to be synthesized, the catalyst operating temperature is controlled to be from 80 to 180 DEG C, and the synthesizing pressure in the synthesizing tower is from 0.2 to 0.8MPa; the mixture discharged from the synthesizing tower is cooled and separated, and separated coarse 3-pentylamine is put into a rectifying tower to be refined to obtain fine 3-pentylamine. The method of the present invention has the advantages that the conversion rate of added materials reaches 99.9%, the 3-pentylamine yield is more than 95%, a new route for synthesizing original drugs of pendimethalin is provided, the original production cost is reduced, and simultaneously, the raw material problem in dye synthesis is solved.
Description
Technical field
The present invention relates to the technology of the synthetic 3-amylamine of a kind of low-pressure process.
Background technology
The 3-amylamine is an intermediate of producing dinitroaniline herbicide pendimethalin (weeding is logical), it also is a kind of raw material of synthetic dyestuff, the general production circuit of pendimethalin is: 3, the 4-xylidine adds propione and hydrogen generates N-(1-ethyl propyl)-3, the nitrated back of 4-xylidine generates pendimethalin, and intermediate is propione and hydrogen.
Summary of the invention
Up to the present, still find no the data of any destruction novelty of the present invention, the inventor by various experiments, test, has obtained best effect, thereby has finished the present invention through studying intensively for many years.
Purpose of the present invention just provides the novel process of the synthetic 3-amylamine of a kind of low-pressure process, reduces production costs.
The present invention is achieved like this, and its synthesis material is propione, liquefied ammonia, hydrogen, and catalyzer is Ni-Cr-HPO
3/ Al
2O
3, adopt following technical process synthetic.
(1) preheating mixes: with propione, liquefied ammonia, hydrogen in molar ratio 0.5～2: 1～5: 2～7 feed intake, and put into the preheating mixer preheating and mix.
(2) synthetic: the mixed raw material of preheating enters and is placed with Ni-Cr-HPO
3/ Al
2O
3The synthetic tower of catalyzer synthesizes, and the catalyzer service temperature is controlled at 80 ℃～180 ℃, and synthesis pressure is 0.2～0.8Mpa in the synthetic tower.
(3) refrigerated separation: the mixture that synthetic tower is come out carries out refrigerated separation, isolated thick 3-amylamine enters rectifying tower, rectifying makes smart 3-amylamine, intact raw material circulation gas propione, gas ammonia, the hydrogen of unreacted after the refrigerated separation, through circulator and oil separator, it is synthetic that processing reenters synthetic tower.
The present invention is a raw material with propione, liquefied ammonia, hydrogen, with Ni-Cr-HPO
3/ Al
2O
3Catalyzer, synthetic under 80 ℃～180 ℃ temperature and 0.2～0.8Mpa, the transformation efficiency that feeds intake reaches 99.9%, the productive rate of 3-amylamine is more than 95%, solve the synthetic new route of the former medicine of pendimethalin, reduce original production cost, solve the synthetic middle raw material problem of dyestuff simultaneously.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Specific implementation method
As shown in Figure 1, consume the raw material quota by 95%3-amylamine per ton, specification is technical grade propione 1.38T/T, liquefied ammonia 0.6T/T, 120 bottles/T of hydrogen, mol ratio is: 1: 3.5: 4.5, feed intake, at first synthesis material is dropped into preheating mixing in the preheating mixer, sending into diameter then is 219 centimetres, high 800 centimetres stainless steel tube synthetic tower synthesizes, and is encased inside Ni-Cr-HPO in the synthetic tower
3/ Al
2O
3Catalyzer, catalyzer service temperature are controlled at 80 ℃～180 ℃, and synthesis pressure is 0.2～0.8Mpa in the synthetic tower.The synthetic mixture that synthetic tower is come out carries out refrigerated separation again, it is refining that the thick 3-amylamine of separating enters rectifying tower, obtain smart 3-amylamine, the raw material circulation gas that unreacted has synthesized enters circulator and oil separator is handled, circulator be 2F-10 refrigerating capacity 2.8 ten thousand kilocalories/hour, it is synthetic that the synthesis material of processing reenters synthetic tower.
Claims (1)
1. a low-pressure process is synthesized 3-amylamine technology, and synthesis material propione, liquefied ammonia, hydrogen, catalyzer are Ni-Cr-HPO
3/ Al
2O
3, it is characterized in that the synthesis technique flow process is as follows:
(1) preheating mixes: with propione, liquefied ammonia, hydrogen in molar ratio 0.5～2: 1～5: 2～7 feed intake, and put into the preheating mixer preheating and mix;
(2) synthetic: the mixed raw material of preheating enters and is placed with Ni-Cr-HPO
3/ Al
2O
3The synthetic tower of catalyzer synthesizes, and the catalyzer service temperature is controlled at 80 ℃～180 ℃, and synthesis pressure is 0.2～0.8Mpa in the synthetic tower;
(3) refrigerated separation: the mixture that synthetic tower is come out carries out refrigerated separation, isolated thick 3-amylamine enters rectifying tower, and rectifying makes smart 3-amylamine, the intact raw material circulation gas of unreacted after the refrigerated separation, through circulator and oil separator, it is synthetic that processing reenters synthetic tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510018354XA CN100395229C (en) | 2005-03-04 | 2005-03-04 | Process for low pressure synthesizing 3-pentylamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510018354XA CN100395229C (en) | 2005-03-04 | 2005-03-04 | Process for low pressure synthesizing 3-pentylamine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1683319A CN1683319A (en) | 2005-10-19 |
| CN100395229C true CN100395229C (en) | 2008-06-18 |
Family
ID=35262846
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200510018354XA Expired - Fee Related CN100395229C (en) | 2005-03-04 | 2005-03-04 | Process for low pressure synthesizing 3-pentylamine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100395229C (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1130621A (en) * | 1995-03-06 | 1996-09-11 | 化学工业部北京化工研究院 | Process for producing isopropyl amine |
| CN1270161A (en) * | 1999-03-12 | 2000-10-18 | 巴斯福股份公司 | Preparation of amine |
| US20010003137A1 (en) * | 1999-12-06 | 2001-06-07 | Jan Nouwen | Process for preparing monoisopropylamine |
| WO2003076386A2 (en) * | 2002-03-14 | 2003-09-18 | Basf Aktiengesellschaft | Catalysts and method for the production of amines |
-
2005
- 2005-03-04 CN CNB200510018354XA patent/CN100395229C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1130621A (en) * | 1995-03-06 | 1996-09-11 | 化学工业部北京化工研究院 | Process for producing isopropyl amine |
| CN1270161A (en) * | 1999-03-12 | 2000-10-18 | 巴斯福股份公司 | Preparation of amine |
| US20010003137A1 (en) * | 1999-12-06 | 2001-06-07 | Jan Nouwen | Process for preparing monoisopropylamine |
| WO2003076386A2 (en) * | 2002-03-14 | 2003-09-18 | Basf Aktiengesellschaft | Catalysts and method for the production of amines |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1683319A (en) | 2005-10-19 |
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Granted publication date: 20080618 Termination date: 20110304 |