CN212451250U - Production system of (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol - Google Patents
Production system of (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol Download PDFInfo
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- CN212451250U CN212451250U CN202020236650.7U CN202020236650U CN212451250U CN 212451250 U CN212451250 U CN 212451250U CN 202020236650 U CN202020236650 U CN 202020236650U CN 212451250 U CN212451250 U CN 212451250U
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Abstract
The utility model discloses a production system of (1R,2R,6S) -2, 6-di tert-butyl-4-methyl cyclohexanol, including hydrogenation cauldron, filter, reduction cauldron, water drip jar, hydrochloric acid dropwise add jar, refined cauldron, condenser and receiving tank. The filter feed inlet of the filter is connected with the hydrogenation kettle discharge outlet of the hydrogenation kettle; the reducing kettle feed inlet of the reducing kettle is connected with the filter discharge outlet of the filter; a water dripping port of the reduction kettle is connected with a water outlet of the water dripping tank; a hydrochloric acid dropping port of the reduction kettle is connected with a hydrochloric acid outlet of the hydrochloric acid dropping tank; the refining kettle feed inlet of the refining kettle is connected with the reducing kettle discharge outlet of the reducing kettle; the steam inlet of the condenser is connected with the steam outlet of the refining kettle; the recovered solvent inlet of the receiving tank is connected with the solvent outlet of the condenser. The utility model discloses a production system reaction is single, and reaction condition is mild, and the security is higher, and production efficiency is higher, and product optical purity is higher.
Description
Technical Field
The utility model relates to a production system of (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol.
Background
The 2, 6-di-tert-butyl-4-methylcyclohexanol can be used as a dispersant in the field of photography, can be used as a solvent in the field of dyes, and can be used as an intermediate in the fields of medicines and pesticides.
At present, the method for producing 2, 6-di-tert-butyl-4-methylcyclohexanol mainly uses di-tert-butyl-4-methylphenol (BHT) as a raw material, and prepares 2, 6-di-tert-butyl-4-methylcyclohexanol through one-step hydrogenation reaction in the presence of a supported catalyst and a solvent, the reaction conditions of the process are severe, long-time reaction under high temperature and high pressure conditions is required, great potential safety hazards exist, and catalytic hydrogenation is difficult to obtain (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol with high optical purity.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to solve above-mentioned problem, provide a reaction is single, reaction condition is mild, the security is higher, especially the higher (1R,2R,6S) -2, 6-di tert-butyl-4-methylcyclohexanol' S of product optical purity production system.
Realize the utility model discloses the technical scheme of purpose is: a production system of (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol is characterized by comprising a hydrogenation kettle, a filter, a reduction kettle, a water dripping tank, a hydrochloric acid dripping tank, a refining kettle, a condenser and a receiving tank.
The hydrogenation kettle is provided with a hydrogenation kettle feeding hole, a hydrogenation kettle air inlet, a hydrogenation kettle air outlet and a hydrogenation kettle discharging hole; the filter is provided with a filter feeding hole, a filter exhaust hole and a filter discharging hole; the reduction kettle is provided with a reduction kettle feeding hole, a water dropping hole, a hydrochloric acid dropping hole, a reduction kettle exhaust hole and a reduction kettle discharge hole; the water dripping tank is provided with a water inlet, a water dripping tank exhaust port and a water outlet; the hydrochloric acid dripping tank is provided with a hydrochloric acid inlet, a hydrochloric acid dripping tank exhaust port and a hydrochloric acid outlet; the refining kettle is provided with a refining kettle feeding hole, a steam outlet, a solvent return port and a refining kettle discharging hole; the condenser is provided with a steam inlet, a solvent outlet, a refrigerant inlet and a refrigerant outlet; and the receiving tank is provided with a recovered solvent inlet, a receiving tank exhaust port and a recovered solvent outlet.
The filter feed inlet of the filter is connected with the hydrogenation kettle discharge outlet of the hydrogenation kettle; the reduction kettle feed inlet of the reduction kettle is connected with the filter discharge outlet of the filter; a water dripping port of the reduction kettle is connected with a water outlet of the water dripping tank; a hydrochloric acid dropping port of the reduction kettle is connected with a hydrochloric acid outlet of the hydrochloric acid dropping tank; the refining kettle feed inlet of the refining kettle is connected with the reduction kettle discharge outlet of the reduction kettle; the steam inlet of the condenser is connected with the steam outlet of the refining kettle; and a recovered solvent inlet of the receiving tank is connected with a solvent outlet of the condenser.
And the solvent outlet of the condenser is connected with the solvent reflux port of the refining kettle.
And a refining kettle discharge port of the refining kettle is also provided with a heat tracing device.
The utility model discloses positive effect that has: the utility model discloses a production system reaction is single, and reaction condition is mild, and the security is higher, and production efficiency is higher, and product optical purity is higher.
Drawings
FIG. 1 is a schematic structural diagram of a production system of (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol of the present invention.
Detailed Description
Referring to fig. 1, the utility model discloses a production system of (1R,2R,6S) -2, 6-di tert-butyl-4-methylcyclohexanol includes hydrogenation cauldron 1, filter 2, reduction kettle 3, water dropwise add jar 4, hydrochloric acid dropwise add jar 5, refined cauldron 6, condenser 7 and receiving tank 8.
The hydrogenation kettle 1 is provided with a hydrogenation kettle feed inlet 11, a hydrogenation kettle air inlet 12, a hydrogenation kettle air outlet 13 and a hydrogenation kettle discharge outlet 14.
The filter 2 is provided with a filter inlet 21, a filter outlet 22 and a filter outlet 23. The filter inlet 21 of the filter 2 is connected with the hydrogenation reactor outlet 14 of the hydrogenation reactor 1.
The reduction kettle 3 is provided with a reduction kettle feed inlet 31, a water dropping port 32, a hydrochloric acid dropping port 33, a reduction kettle exhaust port 34 and a reduction kettle discharge port 35. The reduction kettle inlet 31 of the reduction kettle 3 is connected with the filter outlet 23 of the filter 2.
The water dropping tank 4 is provided with a water inlet 41, a water dropping tank exhaust port 42 and a water outlet 43. The hydrochloric acid dripping tank 5 is provided with a hydrochloric acid inlet 51, a hydrochloric acid dripping tank exhaust port 52 and a hydrochloric acid outlet 53. The water dropping port 32 of the reduction kettle 3 is connected with the water outlet 43 of the water dropping tank 4. The hydrochloric acid dropping port 33 of the reduction kettle 3 is connected with the hydrochloric acid outlet 53 of the hydrochloric acid dropping tank 5.
The refining kettle 6 is provided with a refining kettle feed inlet 61, a steam outlet 62, a solvent return inlet 63 and a refining kettle discharge outlet 64. The refining kettle feed inlet 61 of the refining kettle 6 is connected with the reducing kettle discharge outlet 35 of the reducing kettle 3. The refining kettle 6 is also provided with a heat tracing device 641 at the outlet 64.
The condenser 7 is provided with a vapor inlet 71, a solvent outlet 72, a refrigerant inlet 73, and a refrigerant outlet 74. The steam inlet 71 of the condenser 7 is connected with the steam outlet 62 of the refining kettle 6; the solvent outlet 72 of the condenser 7 is connected to the solvent reflux port 63 of the purification vessel 6.
The receiver tank 8 is provided with a recovered solvent inlet 81, a receiver tank vent 82, and a recovered solvent outlet 83. The recovered solvent inlet 81 of the receiver tank 8 is connected to the solvent outlet 72 of the condenser 7.
The process comprises the following steps: firstly, carrying out catalytic hydrogenation on 2, 6-di-tert-butyl-4-methylphenol in a hydrogenation kettle to obtain an intermediate 2, 6-di-tert-butyl-4-methylcyclohexanone, carrying out reduction reaction on the intermediate in a reduction kettle by using sodium borohydride as a reducing agent and Lewis acid as a catalyst, then dripping water and hydrochloric acid at a certain temperature for layering, refining and purifying the material in a refining kettle, and concentrating the solvent to obtain (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol.
The reaction route is as follows:
because the melting point of (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol is higher, a heat tracing device is arranged at a refining kettle discharge port 64 of the refining kettle 6 to prevent the materials from condensing and blocking a pipeline.
Claims (3)
1. A production system of (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol is characterized by comprising a hydrogenation kettle (1), a filter (2), a reduction kettle (3), a water dropping tank (4), a hydrochloric acid dropping tank (5), a refining kettle (6), a condenser (7) and a receiving tank (8);
the hydrogenation kettle (1) is provided with a hydrogenation kettle feeding port (11), a hydrogenation kettle air inlet (12), a hydrogenation kettle air outlet (13) and a hydrogenation kettle discharging port (14);
the filter (2) is provided with a filter feeding hole (21), a filter exhaust hole (22) and a filter discharging hole (23);
the reduction kettle (3) is provided with a reduction kettle feeding hole (31), a water dropping hole (32), a hydrochloric acid dropping hole (33), a reduction kettle exhaust hole (34) and a reduction kettle discharge hole (35);
the water dripping tank (4) is provided with a water inlet (41), a water dripping tank exhaust port (42) and a water outlet (43);
the hydrochloric acid dripping tank (5) is provided with a hydrochloric acid inlet (51), a hydrochloric acid dripping tank exhaust port (52) and a hydrochloric acid outlet (53);
the refining kettle (6) is provided with a refining kettle feeding hole (61), a steam outlet (62), a solvent return hole (63) and a refining kettle discharging hole (64);
the condenser (7) is provided with a steam inlet (71), a solvent outlet (72), a refrigerant inlet (73) and a refrigerant outlet (74);
the receiving tank (8) is provided with a recovered solvent inlet (81), a receiving tank exhaust port (82) and a recovered solvent outlet (83);
a filter feeding hole (21) of the filter (2) is connected with a hydrogenation kettle discharging hole (14) of the hydrogenation kettle (1);
a reducing kettle feeding hole (31) of the reducing kettle (3) is connected with a filter discharging hole (23) of the filter (2);
a water dripping port (32) of the reduction kettle (3) is connected with a water outlet (43) of the water dripping tank (4);
a hydrochloric acid dripping port (33) of the reduction kettle (3) is connected with a hydrochloric acid outlet (53) of the hydrochloric acid dripping tank (5);
a refining kettle feed inlet (61) of the refining kettle (6) is connected with a reducing kettle discharge outlet (35) of the reducing kettle (3);
a steam inlet (71) of the condenser (7) is connected with a steam outlet (62) of the refining kettle (6);
the recovered solvent inlet (81) of the receiving tank (8) is connected with the solvent outlet (72) of the condenser (7).
2. The production system of (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol according to claim 1, characterized in that: and a solvent outlet (72) of the condenser (7) is connected with a solvent reflux port (63) of the refining kettle (6).
3. The production system of (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol according to claim 1, characterized in that: and a heat tracing device (641) is also arranged at the refining kettle discharge port (64) of the refining kettle (6).
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CN202020236650.7U CN212451250U (en) | 2020-02-29 | 2020-02-29 | Production system of (1R,2R,6S) -2, 6-di-tert-butyl-4-methylcyclohexanol |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115677454A (en) * | 2022-11-15 | 2023-02-03 | 山东重山光电材料股份有限公司 | Preparation method and device of high-purity perfluoro-tert-butyl alcohol |
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2020
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115677454A (en) * | 2022-11-15 | 2023-02-03 | 山东重山光电材料股份有限公司 | Preparation method and device of high-purity perfluoro-tert-butyl alcohol |
CN115677454B (en) * | 2022-11-15 | 2024-04-02 | 山东重山光电材料股份有限公司 | Preparation method and device of high-purity perfluoro-tert-butanol |
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