CN101962316B - Manufacturing method of granular potassium tert-pentylate - Google Patents
Manufacturing method of granular potassium tert-pentylate Download PDFInfo
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- CN101962316B CN101962316B CN 201010510581 CN201010510581A CN101962316B CN 101962316 B CN101962316 B CN 101962316B CN 201010510581 CN201010510581 CN 201010510581 CN 201010510581 A CN201010510581 A CN 201010510581A CN 101962316 B CN101962316 B CN 101962316B
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- amyl alcohol
- tertiary amyl
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Abstract
The invention discloses a manufacturing method of granular potassium tert-pentylate, comprising the following steps: taking potassium metal, tert-amyl alcohol and inert organic solvent as raw materials; adding tert-amyl alcohol and inert organic solvent into a kettle; then, adding potassium metal into the kettle; after reflowing for 8-40 hours under the protection of nitrogen, evaporating tert-amyl alcohol at normal pressure; after tert-amyl alcohol is completely evaporated, decompressing to -0.08--0.098 MPa, and evaporating residual organic solvent; then, regulating the stirring rate of the kettle to 10-80 turns/min; decompressing to evaporate inert organic solvent, and leaving granular potassium tert-pentylate products in the kettle; and cooling to be below 40 DEG C to obtain the granular potassium tert-pentylate. The invention can carry out production by using general chemical equipment, has moderate operation condition, simple production technology, convenient and abundant raw material, and stable and reliable product quality and can effectively prolong the quality guarantee period of the product.
Description
Technical field
The present invention relates to a kind of manufacture method of fine-chemical intermediate, particularly relate to a kind of manufacture method of particulate state tertiary amyl alcohol potassium.
Background technology
Tertiary amyl alcohol potassium is a kind of intermediate of widespread use in fine chemistry industry, is usually used in etherificate, esterification, and the various reactions of carbonyl α position, for the manufacture of products such as medicine and dyestuffs.Tertiary amyl alcohol potassium product commonly used is powdery substance, because the severe corrosive of this product, strong water absorbability, the dust that produces in operation feeds intake causes very big infringement to operator ' s health, and the inflammable and explosive characteristics of dust also threaten to the safety of production environment in addition.For human injury and the safety problem that prevents that tertiary amyl alcohol potassium powder from causing, the solution of usually tertiary amyl alcohol potassium being made toluene uses, and still brings inconvenience to the user but in use need remove solvent.Because the hazardness of tertiary amyl alcohol potassium dust needs a kind of technology simple, the industrialization technology of tertiary amyl alcohol potassium being made granular product that can large-scale production makes this product can obtain safely using, and is the urgent task of these those skilled in the art at present.
Summary of the invention
The objective of the invention is to: the method that a kind of tertiary amyl alcohol of production particulate state easily potassium is provided.
The manufacture method of particulate state tertiary amyl alcohol potassium is characterized in that, comprises the steps:
Be raw material with potassium metal, tertiary amyl alcohol, inert organic solvents; tertiary amyl alcohol, inert solvent are dropped in the reactor; again potassium metal is dropped in the reactor; after refluxing 8～40 hours under the nitrogen protection; steam tertiary amyl alcohol under the normal pressure; treat that tertiary amyl alcohol steams to the greatest extent; be decompressed to-0.08～-0.098MPa; residual inert organic solvents is steamed; conditioned reaction still stir speed (S.S.) to 10～80 rev/min then; decompression steams inert organic solvents, and residual particles shape tertiary amyl alcohol potassium product in the still is cooled to and namely gets required particulate state tertiary amyl alcohol potassium below 40 ℃.
Count in molar ratio, the mol ratio of described potassium metal and tertiary amyl alcohol is 1: 1.2～10, be preferably 1: 1.2～and 2.0.
By weight, the weight ratio of described tertiary amyl alcohol and inert organic solvents is 1: 0.5～50, be preferably 1: 2.0～and 3.0.
Described inert organic solvents is: 1,2,4-trimethylbenzene, 1,3,5-trimethylbenzene, 1,2,3-trimethylbenzene, p-Diethylbenzene, adjacent diethylbenzene, at least a in NSC 62102 and composition thereof is preferably 1,2, the 4-trimethylbenzene, the mixture of 1,3,5-trimethylbenzene and 1.
The described reaction times is preferably 12～24 hours.
The preferred rotating speed of described reactor stir speed (S.S.) is preferably 8～20 rev/mins.
Beneficial effect of the present invention is: granular tertiary amyl alcohol potassium can effectively solve powdery tertiary amyl alcohol potassium to the harm of operator's health, reduce the production environment security risk, the present invention utilizes the universalization construction equipment to produce, operational condition is gentle, production technique is simple, use raw material conveniently to be easy to get, stable and reliable product quality can effectively prolong quality guaranteed period of product.
Embodiment
The present invention is further described below in conjunction with specific embodiment:
Embodiment 1
In the four-hole reaction flask of dry 2000ml; mechanical stirring is housed; thermometer; charging opening, reflux exchanger adds tertiary amyl alcohol 238g (2.77mol); mix trimethylbenzene 477g; potassium metal fritter 90g (2.31mol), under nitrogen protection, back flow reaction 10 hours; the potassium metal completely dissolve; use water distilling apparatus instead, normal pressure steams excessive tertiary amyl alcohol, steams residual mixing trimethylbenzene under vacuum-0.095MPa; keep 20 rev/mins of speed of rotating speed to stir; when mixing trimethylbenzene and steam to the greatest extent, produce about 0.6mm evenly the tertiary amyl alcohol k particle in the bottle and be blown into low temperature nitrogen (20 ℃) by the reactor bottom valve and reach and be cooled to below 40 ℃, namely get required particulate state tertiary amyl alcohol potassium.
Embodiment 2
The reactor of dry 2000L; add tertiary amyl alcohol 238kg (2.77kmol); mix trimethylbenzene 477kg; drop into potassium metal piece 90kg (2.31kmol) under the nitrogen protection; thrown the rear enclosed reactor; back flow reaction is 14 hours under nitrogen protection; normal pressure steams excessive tertiary amyl alcohol; steam residual mixing trimethylbenzene under vacuum-0.098MPa, keep 20 rev/mins of stir speed (S.S.)s of rotating speed, after mixing trimethylbenzene steaming to the greatest extent; reacting kettle jacketing is introduced water quench; be blown into nitrogen (20 ℃) for several times from still bottom valve gap simultaneously, be cooled to 38 ℃ after, namely getting granularity is 0.4mm particle tertiary amyl alcohol potassium.
Embodiment 3
The reactor of dry 2000L; add tertiary amyl alcohol 397kg (4.62kmol); mix trimethylbenzene 1191kg; drop into potassium metal piece 90kg (2.31kmol) under the nitrogen protection; thrown the rear enclosed reactor; back flow reaction is 14 hours under nitrogen protection; normal pressure steams excessive tertiary amyl alcohol; steam residual mixing trimethylbenzene under vacuum-0.098MPa, keep 20 rev/mins of stir speed (S.S.)s of rotating speed, after mixing trimethylbenzene steaming to the greatest extent; reacting kettle jacketing is introduced water quench; be blown into nitrogen (20 ℃) for several times from still bottom valve gap simultaneously, be cooled to 38 ℃ after, namely getting granularity is 0.4mm particle tertiary amyl alcohol potassium.
Embodiment 4
The reactor of dry 2000L; add tertiary amyl alcohol 318kg (3.70kmol); mix trimethylbenzene 795kg; drop into potassium metal piece 90kg (2.31kmol) under the nitrogen protection; thrown the rear enclosed reactor; back flow reaction is 14 hours under nitrogen protection; normal pressure steams excessive tertiary amyl alcohol; steam residual mixing trimethylbenzene under vacuum-0.098MPa, keep 20 rev/mins of stir speed (S.S.)s of rotating speed, after mixing trimethylbenzene steaming to the greatest extent; reacting kettle jacketing is introduced water quench; be blown into nitrogen (20 ℃) for several times from still bottom valve gap simultaneously, be cooled to 38 ℃ after, namely getting granularity is 0.4mm particle tertiary amyl alcohol potassium.
Embodiment 5
The reactor of dry 2000L; add tertiary amyl alcohol 318kg (3.70kmol); mix trimethylbenzene 636kg; drop into potassium metal piece 90kg (2.31kmol) under the nitrogen protection; thrown the rear enclosed reactor; back flow reaction is 15 hours under nitrogen protection; normal pressure steams excessive tertiary amyl alcohol; steam residual mixing trimethylbenzene under vacuum-0.098MPa, keep 20 rev/mins of stir speed (S.S.)s of rotating speed, after mixing trimethylbenzene steaming to the greatest extent; reacting kettle jacketing is introduced water quench; be blown into nitrogen (20 ℃) for several times from still bottom valve gap simultaneously, be cooled to 38 ℃ after, namely getting granularity is 0.4mm particle tertiary amyl alcohol potassium.
Claims (6)
1. the manufacture method of particulate state tertiary amyl alcohol potassium is characterized in that, comprises the steps:
Be raw material with potassium metal, tertiary amyl alcohol, inert organic solvents, tertiary amyl alcohol, inert solvent are dropped in the reactor, again potassium metal is dropped in the reactor, after refluxing 8～40 hours under the nitrogen protection, steam tertiary amyl alcohol under the normal pressure, treat that tertiary amyl alcohol steams to the greatest extent, be decompressed to-0.08～-0.098MPa, residual inert organic solvents is steamed, conditioned reaction still stir speed (S.S.) to 10～80 rev/min then, decompression steams inert organic solvents, and residual particles shape tertiary amyl alcohol potassium product in the still is cooled to and namely gets required particulate state tertiary amyl alcohol potassium below 40 ℃;
The mol ratio of described potassium metal and tertiary amyl alcohol is 1: 1.2～10;
The weight ratio of described tertiary amyl alcohol and inert organic solvents is 1: 0.5～50;
Described inert solvent is: 1,2,4-trimethylbenzene, 1,3,5-trimethylbenzene, 1, p-Diethylbenzene, adjacent diethylbenzene, at least a in NSC 62102 and composition thereof.
2. according to the manufacture method of right 1 described particulate state tertiary amyl alcohol potassium, it is characterized in that: the described reaction times is preferably 12～24 hours.
3. according to the manufacture method of right 1 described particulate state tertiary amyl alcohol potassium, it is characterized in that: the preferred rotating speed of described reactor stir speed (S.S.) is preferably 8～20 rev/mins.
4. according to the manufacture method of right 2 described particulate state tertiary amyl alcohol potassium, it is characterized in that: described meter in molar ratio, the mol ratio of described potassium metal and tertiary amyl alcohol is preferably 1: 1.2～and 2.0.
5. according to the manufacture method of right 3 described particulate state tertiary amyl alcohol potassium, it is characterized in that: the weight ratio of described tertiary amyl alcohol and inert organic solvents is preferably 1: 2.0～and 3.0.
6. according to the manufacture method of right 4 described particulate state tertiary amyl alcohol potassium, it is characterized in that: described inert organic solvents is preferably 1,2,4-trimethylbenzene, the mixture of 1,3,5-trimethylbenzene and 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010510581 CN101962316B (en) | 2010-10-19 | 2010-10-19 | Manufacturing method of granular potassium tert-pentylate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010510581 CN101962316B (en) | 2010-10-19 | 2010-10-19 | Manufacturing method of granular potassium tert-pentylate |
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| CN101962316A CN101962316A (en) | 2011-02-02 |
| CN101962316B true CN101962316B (en) | 2013-08-14 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105254472A (en) * | 2015-09-02 | 2016-01-20 | 山东朗恒化学有限公司 | Preparation method for low residual granular sodium alkoxide or potassium alcoholate |
| CN105669374B (en) * | 2016-01-15 | 2017-10-31 | 绍兴上虞华伦化工有限公司 | A kind of synthetic method of lithium methoxide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1227212A (en) * | 1998-01-21 | 1999-09-01 | 希尔斯股份公司 | Process for preparing low and high grade alkali metal alcohol salts, particularly tertiary potassium butoxide |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1227212A (en) * | 1998-01-21 | 1999-09-01 | 希尔斯股份公司 | Process for preparing low and high grade alkali metal alcohol salts, particularly tertiary potassium butoxide |
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Owner name: CHANGZHOU GENCHEM + GENPHARM PHARMACEUTICAL CO., L Free format text: FORMER NAME: CHANGZHOU JIEN CHEMICAL CO.,LTD. |
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Address after: 213127 No. 658 ERON North Road, Xinbei District, Jiangsu, Changzhou Patentee after: GENCHEM & GENPHARM (CHANGZHOU) CO., LTD. Address before: 213127, Changzhou, Hebei Province, North Riverside chemical industry park, Binjiang Road, No. 8 Changzhou Jiangsu Chemical Co., Ltd. Patentee before: Changzhou Jien Chemical Co.,Ltd. |