CN105622436A - Preparation method of 6-amino-1-hexanol by taking calcium carbonate as catalyst - Google Patents
Preparation method of 6-amino-1-hexanol by taking calcium carbonate as catalyst Download PDFInfo
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- CN105622436A CN105622436A CN201610114746.4A CN201610114746A CN105622436A CN 105622436 A CN105622436 A CN 105622436A CN 201610114746 A CN201610114746 A CN 201610114746A CN 105622436 A CN105622436 A CN 105622436A
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- calcium carbonate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
Abstract
The invention discloses a preparation method of 6-amino-1-hexanol by taking calcium carbonate as a catalyst. Calcium carbonate serves as the catalyst of a reaction, 1,6-hexanediol, ammonia and hydrogen are mixed and react for 1.5-2 h in a heated and pressurized mode on the condition that the temperature ranges from 270 DEG C to 290 DEG C, and the pressure ranges from 150 Mpa to 180 Mpa, and 6-amino-1-hexanol is generated. According to the preparation method, calcium carbonate serves as the catalyst, the raw materials are easy to obtain, the cost is low, the catalytic efficiency is high, and the catalytic effect is stable; the finished product 6-amino-1-hexanol is high in purity and high in yield, the high economic benefit is achieved, and the preparation method can be widely applied and promoted.
Description
Technical field:
The present invention relates to a kind of take calcium carbonate as the own alcohol preparation method of 6-amino-1-of catalyzer, and the method take calcium carbonate as catalyzer.
Background technology:
The own alcohol of 6-amino-1-, English name is 6-amino-1-hexanol, and No. CAS is 4048-33-3, and molecular formula is C6H16NO, being white, needle-shaped crystals under room temperature, fusing point is 58-60 DEG C, and boiling point is 130.5-131.5 DEG C, air seasoning place, sealing preserves, and is with irritant. The own alcohol of 6-amino-1-is a kind of chemical intermediate, and it contains hydroxyl and amino, has the general character of alkohol and amine, can be used for preparing extraordinary organic chemicals, medicine and agricultural chemicals, and purposes is extensive.
China is relatively backward for 6-amino-1-own alcohol production technology, and great majority rely on import, expensive.
The method producing the 6-own alcohol of amino-1-in currently available technology has multiple, wherein 1,6-HD and ammonia react method, and raw material is easy to get, and product cost is low, has higher industrial prospect.
The reaction equation of 1,6-HD and ammonia react method is:
HOCH2(CH2)4CH2OH+NH3��H2NCH2(CH2)4CH2OH+H2O
This method is divided into again two kinds according to catalyzer difference.
The first nickel makes catalyzer. Raney nickel sodium sulfite solution processes, and obtains the nickel catalyzator containing sulphur. Under this kind of catalyzer exists, 1,6-HD, ammonia heating and pressurizing together with hydrogen, at 210 DEG C and 47kg/cm2Lower reaction 2.5h, generates this alcohol. The own alcohol selectivity 79% of 1,6-HD transformation efficiency 42%, 6-amino-1-.
Catalyzer made by 2nd kind of iron. Under iron catalyst exists, under 150-300 DEG C and 50-200 handkerchief pressure, there is light base, amide exchange reaction in l, 6-hexylene glycol and ammonia, generates the 6-own alcohol of amino-1-.
But the catalytic efficiency of 1,6-HD and ammonia react its catalyzer of method is all not ideal at present, and receipts rate is on the low side.
Summary of the invention:
Technical problem solved by the invention:
There is provided a kind of 1,6-HD and the effective catalyst of ammonia react method, it is to increase the receipts rate of the own alcohol of 6-amino-1-and purity.
The present invention provides following technical scheme:
The preparation method of a kind of 6-own alcohol of amino-1-taking calcium carbonate as catalyzer, take calcium carbonate as catalysts, by 1,6-HD, ammonia and hydrogen temperature be 270-290 DEG C, pressure within Hybrid Heating compressive reaction 1.5-2 hour, generate 6-amino-1-own alcohol when being 150-180Mpa.
Preferably, take calcium carbonate as catalysts, by 1,6-HD, ammonia and hydrogen temperature be 280-290 DEG C, pressure within Hybrid Heating compressive reaction 1.5-2 hour, generate 6-amino-1-own alcohol when being 170-180Mpa.
Preferably, take calcium carbonate as catalysts, by 1,6-HD, ammonia and hydrogen temperature be 280-285 DEG C, pressure within Hybrid Heating compressive reaction 1.5-2 hour, generate 6-amino-1-own alcohol when being 170-175Mpa.
Preferably, described calcium carbonate is activated Calcium carbonate, CaCO3 active constituent content >=98%, Fe2O3 content��0.30%, Al2O3 content��0.20%, content of MgO��0.16%.
Preferably, described calcium carbonate is calcium carbonate superfine powder, CaCO3 active constituent content >=96%, iron level��0.1%, MgCO3 content��1.7%, hydrochloric acid insoluble substance content��0.2.
Preferably, described calcium carbonate is ultra-fine calcite in powder, CaCO3 active constituent content >=98%, iron level��0.1%, Fe content��0.008%.
Calcium carbonate is white fine crystalline powder, and odorless, tasteless, can absorb foul smell, and relative density is 2.6-2.7g/cm3; Relative steam density is 2.5-2.74g/cm3, and fusing point is 1339 DEG C; Specific refractory power: 1.498, dissolves in the diluted acid such as acetic acid, hydrochloric acid, is insoluble in dilute sulphuric acid, is almost insoluble to water and ethanol, and thermal linear expansion coefficient is 11.7 �� 10-6 DEG C.
Light calcium carbonate can be used as raising agent, Flour ingredient, anticaking agent, acidity regulator, nutrition-fortifying agent, solidifying agent etc. This product do when raising agent uses many with other kinds with the use of, the raising agent that obtain composite with sodium bicarbonate, alum etc., heat then disengages carbonic acid gas slowly, makes food produce even, fine and smooth bulk body, can improve the quality of cake, bread, biscuit. In addition the effect also having strengthening calcium, calcium carbonate granule is more little more easily absorbs. Feed nutrition reinforcer and chemical industry weighting agent can also be used as, in rubber industry, extensively in sebific duct, offset plate, adhesive plaster, rubber overshoes and medical article, it is the good filler reducing goods cost. In plastics industry, being mainly used in flexible PVC mixture, the aspects such as plastisol and glass-fiber-reinforced polyester mixture, such as wire outer skin, leatheroid and other extrusion calendered goods, general consumption is about 20 parts. Calcium carbonate is used as analytical reagent, as made standard reagent. Sample fusing assistant, volatile aids in emmission spectrometric analysis. Also it is used as silicon single-crystal section glue, thick film capacitance material, opticglass and medicine industry raw material. Calcium carbonate, for the manufacture of raw materials such as face powder, muffin, pigment, kermes, is used as essence mixture, is also mainly used in toothpaste and makes friction agent, belong to the rigid abrasive material of toothpaste when manufacturing powder class makeup.
Without any can as the record of chemical catalyst about calcium carbonate in prior art, the present invention adopts calcium carbonate to be 1,6-HD and ammonia react catalyzer, catalytic efficiency height, catalytic effect is stablized, calcium carbonate wide material sources, simple and easy to get, there is extremely high market popularization value.
The useful effect of the present invention:
1. 1,6-HD of the present invention and ammonia react raw material are easy to get, and product cost is low, good in economic efficiency.
2. adopting calcium carbonate to be 1,6-HD and ammonia react catalyzer, catalytic efficiency height, catalytic effect is stablized, finished product purity height, receipts rate height.
3. calcium carbonate is low as catalyst economy cost, and raw material is easy to get, it is possible to wide popularization and application.
Embodiment:
Being described in detail by embodiments of the invention below, the present embodiment is implemented under premised on inventive technique scheme, gives detailed enforcement mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment. The experimental program of unreceipted concrete condition in embodiment, the condition that conveniently condition or manufacturers advise usually is implemented.
Embodiment
The preparation method of a kind of 6-own alcohol of amino-1-taking calcium carbonate as catalyzer, take calcium carbonate as catalysts, by 1,6-HD, ammonia and hydrogen temperature be 270-290 DEG C, pressure within Hybrid Heating compressive reaction 1.5-2 hour, generate 6-amino-1-own alcohol when being 150-180Mpa.
Catalyzer one: activated Calcium carbonate, purchased from Hua Yu nano-powder group, CaCO3 active constituent content >=98%, Fe2O3 content��0.30%, Al2O3 content��0.20%, content of MgO��0.16%.
Catalyzer two: calcium carbonate superfine powder, purchased from Hua Yu nano-powder group, CaCO3 active constituent content >=96%, iron level��0.1%, MgCO3 content��1.7%, hydrochloric acid insoluble substance content��0.2.
Catalyzer three: ultra-fine calcite in powder, purchased from Hua Yu nano-powder group, CaCO3 active constituent content >=98%, iron level��0.1%, Fe content��0.008%.
Comparative catalyst one: containing the nickel catalyzator of sulphur.
Comparative catalyst two: iron catalyst.
Enforcement mode is in table one:
1,6-HD transformation efficiency and the generation own alcohol purity of 6-amino-1-to method described in embodiment measure.
Table two: embodiment 1,6-HD transformation efficiency and the generation own alcohol purity of 6-amino-1-
Above content is only the better embodiment of the present invention, for the those of ordinary skill of this area, according to the thought of the present invention, all will change in specific embodiments and applications, and this description should not be construed as limitation of the present invention.
Claims (6)
1. one kind take calcium carbonate as the own alcohol preparation method of 6-amino-1-of catalyzer, it is characterized in that: take calcium carbonate as catalysts, by 1,6-HD, ammonia and hydrogen temperature be 270-290 DEG C, pressure within Hybrid Heating compressive reaction 1.5-2 hour, generate 6-amino-1-own alcohol when being 150-180Mpa.
2. the preparation method of a kind of 6-own alcohol of amino-1-taking calcium carbonate as catalyzer according to claim 1, it is characterized in that: take calcium carbonate as catalysts, by 1,6-HD, ammonia and hydrogen temperature be 280-290 DEG C, pressure within Hybrid Heating compressive reaction 1.5-2 hour, generate 6-amino-1-own alcohol when being 170-180Mpa.
3. the preparation method of a kind of 6-own alcohol of amino-1-taking calcium carbonate as catalyzer according to claim 1, it is characterized in that: take calcium carbonate as catalysts, by 1,6-HD, ammonia and hydrogen temperature be 280-285 DEG C, pressure within Hybrid Heating compressive reaction 1.5-2 hour, generate 6-amino-1-own alcohol when being 170-175Mpa.
4. it is the preparation method of the 6-own alcohol of amino-1-of catalyzer taking calcium carbonate according to a kind of one of claims 1 to 3 Suo Shu, it is characterised in that: described calcium carbonate is activated Calcium carbonate, CaCO3Active constituent content >=98%, Fe2O3Content��0.30%, Al2O3Content��0.20%, content of MgO��0.16%.
5. it is the preparation method of the 6-own alcohol of amino-1-of catalyzer taking calcium carbonate according to a kind of one of claims 1 to 3 Suo Shu, it is characterised in that: described calcium carbonate is calcium carbonate superfine powder, CaCO3Active constituent content >=96%, iron level��0.1%, MgCO3 content��1.7%, hydrochloric acid insoluble substance content��0.2.
6. it is the preparation method of the 6-own alcohol of amino-1-of catalyzer taking calcium carbonate according to a kind of one of claims 1 to 3 Suo Shu, it is characterised in that: described calcium carbonate is ultra-fine calcite in powder, CaCO3Active constituent content >=98%, iron level��0.1%, Fe content��0.008%.
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| CN201610114746.4A CN105622436A (en) | 2016-03-01 | 2016-03-01 | Preparation method of 6-amino-1-hexanol by taking calcium carbonate as catalyst |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB747841A (en) * | 1952-12-12 | 1956-04-18 | Du Pont | Manufacture of aliphatic diamines |
| CN1186453A (en) * | 1995-06-02 | 1998-07-01 | 陶氏化学公司 | Catalyst and process for producing amides |
| CN101121666A (en) * | 2006-08-11 | 2008-02-13 | 小仓合成工业株式会社 | Process for producing amino compound |
-
2016
- 2016-03-01 CN CN201610114746.4A patent/CN105622436A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB747841A (en) * | 1952-12-12 | 1956-04-18 | Du Pont | Manufacture of aliphatic diamines |
| CN1186453A (en) * | 1995-06-02 | 1998-07-01 | 陶氏化学公司 | Catalyst and process for producing amides |
| CN101121666A (en) * | 2006-08-11 | 2008-02-13 | 小仓合成工业株式会社 | Process for producing amino compound |
Non-Patent Citations (4)
| Title |
|---|
| ALFONS BAIKER等: "Catalytic Synthesis of Higher Aliphatic Amines from the Corresponding Alcohols", 《CATAL. REV, -SCI. ENG .》 * |
| 任夫健: "6-氨基-1-己醇合成工艺进展", 《精细与专用化学品》 * |
| 李秋小，张高勇: "脂肪醇催化胺化制叔胺工艺技术现状及前景", 《日用化学工业》 * |
| 杨志钢等: "醇催化胺化反应的研究进展", 《化工科技市场》 * |
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Application publication date: 20160601 |