CN1093352A

CN1093352A - The manufacture method of 2-phenyl-2-propyl alcohol

Info

Publication number: CN1093352A
Application number: CN 93104129
Authority: CN
Inventors: 黄国生; 梁永民; 宋庆宝; 马永祥
Original assignee: Lanzhou University
Current assignee: Lanzhou University
Priority date: 1993-03-31
Filing date: 1993-03-31
Publication date: 1994-10-12
Anticipated expiration: 2013-03-31
Also published as: CN1051541C

Abstract

The invention provides the manufacture method of a kind of 2-phenyl-2-propyl alcohol.2-phenyl-2-propyl alcohol is the suitability for industrialized production dicumyl peroxide important intermediate of (being called for short DCP).Provided by the inventionly reduce method that isopropyl benzene hydroperoxide (CHP) makes 2-phenyl-2-propyl alcohol with sulfide to have a reductive agent cheap and easy to get and consumption is few, reduction reaction speed fast, transformation efficiency and recovery rate height, easily-controlled reaction conditions, equipment is simple and utilization ratio, advantage such as saltiness is low in the sewage, can reduce production costs greatly, increase economic efficiency, reduce and pollute, be fit to very much suitability for industrialized production.

Description

The manufacture method of 2-phenyl-2-propyl alcohol

The invention belongs to organic chemistry compound probability field.

2-phenyl-2-propyl alcohol is the synthetic dicumyl peroxide important source material of (being called for short DCP), and the synthetic method of existing 2-phenyl-2-propyl alcohol is reduced isopropyl benzene hydroperoxide (being called for short CHP) and realized that its reaction equation is as follows with sodium sulfite aqueous solution:

It is more expensive that this production method exists reductive agent S-WAT Jie lattice, large usage quantity (1 molecule S-WAT can only reduce 1 molecule CHP), reductive agent solubleness in water is less, the more high shortcoming of saltiness in reduction reaction late phase reaction speed slow (being that the reaction times is longer) and the waste water.

Day disclosure special permission communique clear 59,110,639, clear 61,246,160 introduce method reduction CHP with catalytic hydrogenation respectively makes 2-phenyl-2-propyl alcohol or portion C HP is reverted to alcohol and directly make DCP without separating, though these methods have the yield height, pollute advantages such as little, must use expensive noble metal catalyst and the conversion unit and the operational condition of complexity.

The present invention introduces a kind of method of making 2-phenyl-2-propyl alcohol with water-soluble sulfide reduction CHP, it is cheap and easy to get to have reductive agent, the reductive agent good water solubility, reduction reaction speed is fast, and (late phase reaction speed is also very fast, residual CHP concentration is low in the reduced liquid), transformation efficiency and recovery rate height, advantage such as reducing process and conversion unit are simple.Compare with the S-WAT reduction method, plant factor obviously improves (promptly use same equipment, can improve its productivity greatly).Because the valency of the sulphur in the sulfide reductive agent that is adopted among the present invention is negative divalence, and the valency of the sulphur in its The product sulfur hydrochlorate after oxidized is positive sexavalence, so a part sulfide can reduce four molecule CHP, therefore saltiness is than S-WAT reduction method reduction more than 70% less and in the waste water for the reductive agent consumption, and its blowdown flow rate can significantly reduce.

Reaction equation with sulfide reduction CHP is as follows:

M in the last reaction formula among the MxS can be H, Li, Na, K, Ca, Mg, NH ₄, X can be 1 or 2.As use H ₂S, NaHS, NH ₄HS etc. make reductive agent, because its oxidation products is acid, are the decomposition that prevents CHP and the dehydration reaction of product alcohol, should in reaction system, add alkali in advance or in reaction process, add continuously alkali with the potential of hydrogen that keeps reaction solution neutral or alkaline.

Relevant key points for operation are as follows:

One, the ingredient proportion of reactant: after single still CHP charging capacity is determined, the M definite according to reaction equation _xThe theoretical consumption of S, the actual amount of sulfide should be no less than theoretical consumption, general M _xThe actual amount of S should surpass 0～200% of theoretical consumption, and it is more suitable to surpass 5-35%.

Two, temperature of reaction, pressure and reaction times: correct adjustable clamp jacket water, jacket steam or utilize reaction heat etc. that reduction reaction temperature is controlled at 0～150 ℃.Pressure is little to this reaction influence, generally is controlled at normal pressure.Reaction times was generally 0.5～8 hour.

Three, aftertreatment: after reduction reaction is finished, with the reactant standing demix, divide the sub-cloud water, organic phase washes with water 1～3 time, gets final product when the PH of washing water is 7～7.2.After washing was finished, organic phase was delivered to vacuum and is carried workshop sections such as dense and condensation.

The present invention has an embodiment as follows:

1.33 kilograms of industrial sodium sulfides (content 〉=60%) are dissolved in 10 liters of hot water, then above-mentioned solution is dropped in the stainless steel cauldron of 30 liters of strap clamp covers and stirrer, open the chuck water coolant, stir down that all the other be isopropyl benzene with 15 kilogram 34.65% CHP() in the solution input reactor, react and stop water coolant after 5 minutes, after making reaction carry out 0.5 hour between 30～35 ℃, the logical small amount of steam of chuck slowly was warming up to 70 ℃ with thing in the still in 0.5 hour, then 70 ± 1 ℃ of following insulation reaction 2 hours.The logical water coolant of chuck makes that material is cooled to about 30 ℃ in the still, stops stirring, and behind the standing demix, separates lower floor's water and a small amount of membranoid substance.Organic phase is washed 2 times with 10 premium on currency at every turn, and ph value of aqueous phase was 7 after washing was finished for the second time.At last 14 kilograms of water white organic liquids.When CHP feeds intake 2 hours and 3 hours (finishing reaction) in the organic phase content of CHP be respectively 0.71% and the 0.385%(iodimetric analysis).2-phenyl in the product-2-propyl alcohol content is the analysis of 30.23%(high pressure lipuid chromatography (HPLC)).

Claims

1, the method for a kind of industrial Synthetic 2-phenyl-2-propyl alcohol is characterized in that (using M with water-soluble sulfide _xS represents) the reactant concn proportioning determined with isopropyl benzene hydroperoxide; The temperature of reaction of determining, reaction times and definite post-treatment condition react down to be finished.

2, a kind of method according to the said industrial Synthetic 2-phenyl of claim 1-2-propyl alcohol, said M _xS is characterized in that: M _xM among the S can be chemical elements such as H, Li, Na, K, Ca, Mg, also can be NH ₄; The number of M in sulfide molecules * can be 1 or 2.

3, a kind of method according to the said industrial Synthetic 2-phenyl of claim 1-2-propyl alcohol, said reactant concn proportioning is characterized in that: M _xThe consumption of S and CHP is determined by reaction equation (specification sheets Chinese style 2).M _xThe consumption of S can feed intake with mole such as CHP, also can be the CHP charging capacity 1-3 doubly.

4, a kind of method according to the said industrial Synthetic 2-phenyl of claim 1-2-propyl alcohol, said temperature of reaction, reaction times, it is characterized in that: temperature of reaction is at 0-150 ℃, and the reaction times is 0.5-8 hour.

5, a kind of method according to the said industrial Synthetic 2-phenyl of claim 1-2-propyl alcohol, said post-treatment condition is characterized in that: after reaction is finished, with the reactant standing demix, divide the sub-cloud water, the pH value that organic phase is washed with water to water is finished aftertreatment during for 6-8.