阅读说明：本技术 一种制备2,6-二叔丁基-4-甲基环己醇的反应工艺 (It is a kind of to prepare 2,6- di-t-butyl -4 methyl cyclohexanol reaction process ) 是由 黄冬 袁俊秀 曾志强 靳志超 于 2018-05-24 设计创作，主要内容包括：一种制备2,6-二叔丁基-4-甲基环己醇的反应工艺,采用固定床反应器中装填两类不同加氢催化剂,以2,6-二叔丁基-4-甲基苯酚为原料一步合成2,6-二叔丁基-4-甲基环己醇。本发明2,6-二叔丁基-4-甲基苯酚的转化率高达99%以上,2,6-二叔丁基-4-甲基环己醇选择性高达98%以上。反应条件温和、反应选择性高、能够实现连续化、反应步骤简单。(It is a kind of to prepare 2,6- di-t-butyl -4 methyl cyclohexanol reaction process, using two class difference hydrogenation catalysts are loaded in fixed bed reactors, with 2,6- di-tert-butyl-4-methy phenol for raw material one-step synthesis 2,6- di-t-butyl -4 methyl cyclohexanol.For the high conversion rate of the present invention 2,6- di-tert-butyl-4-methy phenol up to 99% or more, 2,6- di-t-butyls -4 methyl cyclohexanol is selectively up to 98% or more.Reaction condition is mild, reaction selectivity is high, can be realized serialization, reaction step is simple.)

1. a kind of prepare 2,6- di-t-butyl -4 methyl cyclohexanol reaction process, it is characterized in that filling in fixed bed reactors Two class difference hydrogenation catalysts are filled out, with 2,6- di-tert-butyl-4-methy phenol for raw material one-step synthesis 2,6- di-t-butyl -4- first Cyclohexanol.

2. reaction process according to claim 1, it is characterised in that reaction step is as follows: (1), by 2,6- di-t-butyl- 4- methylphenol is mixed in proportion with solvent；(2), by uniformly mixed material injection two class difference hydrogenation catalysts of filling Fixed bed reactors, a step obtain 2,6- di-t-butyl -4 methyl cyclohexanol crude product；(3), crude product is after being evaporated under reduced pressure except solvent Obtain 2,6- di-t-butyl -4 methyl cyclohexanol.

3. reaction process according to claim 2, it is characterised in that the solvent is methanol, ethyl alcohol and isopropanol.

4. reaction process according to claim 2, it is characterised in that the solvent ratios are 40 ~ 70%wt.

5. reaction process according to claim 2, it is characterised in that in step 2, reaction temperature is 110 ~ 210 DEG C, reaction Pressure is 2 ~ 10MPa.

6. reaction process according to claim 2, it is characterised in that in step 2, hydrogen phenol molar ratio 40 ~ 100, volume sky 0.1 ~ 1.5h of speed^-1。

7. reaction process according to claim 1, it is characterised in that described catalyst one kind is Ni/Al₂O₃, another kind of is Ru/ Al₂O₃Or Rh/Al₂O₃Catalyst.

8. reaction process according to claim 6, it is characterised in that Ni/Al₂O₃Catalyst, 20 ~ 45%wt of Ni content.

9. reaction process according to claim 6, it is characterised in that Ru/Al₂O₃Catalyst, 2.5 ~ 6%wt of Ru content.

10. reaction process according to claim 6, it is characterised in that Rh/A_l2O3Catalyst, 2.5 ~ 6%wt of Rh content.

Technical field

The invention belongs to field of fine chemical, are related to 2,6- of one kind di-t-butyl -4 methyl cyclohexanol reaction process.

Background technique

2,6- di-t-butyl -4 methyl cyclohexanol is mainly used in the fields such as photography, printing and dyeing and medical intermediate.As in Mesosome is used for colour phhotograpy technology as dispersing agent；Field of printing and dyeing is used for as solvent；It is also used as medicine intermediate simultaneously It is used with pesticide intermediate.Currently, mainly adding hydrogen to prepare 2,6- di-t-butyl -4 methyl cyclohexanol using autoclave, with two tertiary fourths Base -4- methylphenol is raw material, under loaded catalyst and solvent existence condition, by adding hydrogen to prepare 2,6- di-t-butyl - 4 methyl cyclohexanol.The technique 2,6- di-t-butyl -4 methyl cyclohexanol selectivity is high, but process conditions are harsh, need in height It is reacted for a long time under temperature, condition of high voltage, and is easy to cause hydrogenolysis, cause post-processing complicated.

EP0703210B prepares 2,6- di-t-butyl -4 methyl cyclohexanol using one-step method.By 0.5%~200% catalyst (mass ratio) and a certain amount of di-tert-butyl-4-methy phenol are added in autoclave simultaneously, at 50 DEG C~300 DEG C of reaction temperature, It is reacted under the conditions of reaction time 12h, 10~25Mpa of reaction pressure, 2, the 6- di-t-butyl-that content is greater than 95% can be obtained 4 methyl cyclohexanol.

EP0720981A1 is related to 2,6- di-t-butyl -4 methyl cyclohexanol preparation method.First by 100g di-t-butyl- 4- methylphenol, 500ml isopropanol, it is 1L into autoclave that 10g Raney's nickel catalyst, which is added to capacity, in reaction temperature It is reacted under the conditions of 100 DEG C, reaction time 9h, reaction pressure 1Mpa, passes through catalyst filtration separation, solvent after reaction Vacuum distillation obtains 2,6- di-t-butyl -4- methyl cyclohexanone；Then by 8.6g lithium aluminium hydride reduction, 200ml tetrahydrofuran is added to In four-hole bottle, 2,6- di-t-butyl -4- methyl cyclohexanone obtained by upper step is slowly added dropwise under 0 DEG C, stirring condition, after being added dropwise It is to slowly warm up to room temperature and maintains room temperature reaction 2h, 40ml methanol is added after reaction and is quenched, hydrochloric acid is added is neutralized, adds Enter the extraction concentration of 600ml ethyl acetate, separating, washing organic phase, vacuum distillation removes solvent and obtains 2,6- di-t-butyl -4- first Cyclohexanol.

US2505817 and US2574078 is related to a kind of preparation method of 2,6- di-t-butyl -4- methyl cyclohexanone.By 10 ~15% Raney's nickel catalyst (mass ratio) and a certain amount of di-tert-butyl-4-methy phenol are added in autoclave, 160 DEG C~ 250 DEG C, reaction time 1h~2h, 10~17Mpa of reaction pressure are reacted to obtain 2,6- di-t-butyl -4- methyl cyclohexanone.

Summary of the invention

It is an object of the invention to overcome that severe reaction conditions exist in the prior art, operating procedure is complicated, can not be continuous Change, the problems such as industrial applications are difficult, a kind of prepares 2,6- di-t-butyl -4 methyl cyclohexanol reaction process to provide.

Main technical schemes of the invention: preparation 2,6- di-t-butyl -4 methyl cyclohexanol reaction process, it is characterized in that Two class difference hydrogenation catalysts are loaded in fixed bed reactors, are the conjunction of one step of raw material with 2,6- di-tert-butyl-4-methy phenol At 2,6- di-t-butyl -4 methyl cyclohexanol.

Generally, reaction step is as follows: (1), by 2,6- di-tert-butyl-4-methy phenol with solvent mixing in proportion It is even；(2), by uniformly mixed material injection two class difference hydrogenation catalyst fixed bed reactors of filling, a step obtains 2,6- bis- Tert-butyl -4 methyl cyclohexanol crude product；(3), crude product obtains 2,6- di-t-butyl -4- methyl cyclohexane after being evaporated under reduced pressure except solvent Alcohol.

The solvent is methanol, ethyl alcohol and isopropanol.

The solvent ratios are 40 ~ 70%wt.

In the step 2, reaction temperature is 110 ~ 210 DEG C, and reaction pressure is 2 ~ 10MPa.

In the step 2, hydrogen phenol molar ratio 40 ~ 100,0.1 ~ 1.5h of volume space velocity^-1。

Described catalyst one kind is Ni/Al₂O₃, another kind of is Ru/Al₂O₃Or Rh/Al₂O₃Catalyst.

The Ni/Al₂O₃Catalyst, 20 ~ 45%wt of Ni content.

The Ru/Al₂O₃Catalyst, 2.5 ~ 6%wt of Ru content.

The Rh/A_l2O3Catalyst, 2.5 ~ 6%wt of Rh content.

Reaction process of the present invention, reaction condition is mild, selectivity is high, it is simple to can be realized serialization, reaction step.2,6- For the high conversion rate of di-tert-butyl-4-methy phenol up to 99% or more, 2,6- di-t-butyls -4 methyl cyclohexanol is selectively up to 98% More than.

Specific embodiment