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A method for preparing odorless isododecane

An isomerized dodecane, odorless technology, applied in the direction of separation methods, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of combustion and explosion, loss of effective components, large consumption, etc., and achieve good adsorption selectivity, The effect of small solid waste output and low regeneration temperature

Active Publication Date: 2021-02-02
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In other technical fields, inorganic adsorbents such as alumina and molecular sieves are generally regenerated by roasting after carbon deposition, but the roasting temperature is relatively high, usually between 350-450 °C, and the requirements for equipment materials are very high. And long-term high temperature treatment will destroy the pore structure of the adsorbent
At the same time, the use of oxygen during roasting is very likely to cause combustion and explosion hazards for the hydrocarbons adsorbed in the adsorbent, especially in olefin hydrogenation devices. Therefore, hot nitrogen or steam must be used for blowing before roasting. Sweep replacement, which requires a large amount of nitrogen and steam consumption, and the water in the steam is extremely detrimental to the stability of the alumina adsorption structure
In addition, the odor substances adsorbed in the adsorbent often only account for a relatively small proportion of the adsorbed materials, and a considerable part is effective products or raw materials, but it is difficult to separate the materials in the pores from the adsorbent during the regeneration process. The materials adsorbed in the adsorbent must be disposed of together, resulting in a large loss of effective components
[0005] In short, it is difficult to solve the contradictions among factors such as three wastes, energy consumption, material consumption, equipment materials and safety when deodorizing products in the production process of isododecane through the existing technology

Method used

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  • A method for preparing odorless isododecane
  • A method for preparing odorless isododecane

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Preparation of porogen: TIB and SO in a falling film sulfonator 3 The sulfonation reaction of TIB with SO 3 The molar ratio is 1:1.1, the sulfonation reaction temperature is 30°C, SO 3 The gas concentration is 5%; the sulfonated product is hydrolyzed with 20wt% NaOH solution at 135°C for 1.5 hours to obtain the sodium sulfonate of TIB.

[0031] Adsorbent preparation: hydrolyze ≥99.99% aluminum isopropoxide at 80°C, add nitric acid while stirring, wherein the molar ratio of aluminum isopropoxide, water and nitric acid is 1:100:0.2. After the solution turns into a transparent sol, add the sodium sulfonate porogen of TIB to it, and the molar ratio of sodium sulfonate to aluminum isopropoxide is 0.05:1. After stirring for 1 hour, put it into a polytetrafluoroethylene-lined autoclave, keep the temperature at 105°C for 24 hours, take it out, cool it and dry it, and then bake it at 500°C for 4 hours to obtain an average particle size of 0.1mm and an average pore size of 2nm....

Embodiment 2

[0037] Preparation of porogen: benzene and TIB with a molar ratio of 1.5:1 are placed in a reactor, and aluminum trichloride equivalent to 1 wt% of the substrate is added as a catalyst, and the reaction is completed at 85°C for 1.5 hours. After quenching by aluminum chloride, the benzene and TIB in the oil phase were removed by distillation, and the obtained dodecylbenzene was treated with SO in the falling film sulfonator. 3 Sulfonated, dodecylbenzene with SO 3 The molar ratio is 1:1.2, the sulfonation reaction temperature is 35°C, SO 3 The gas concentration is 5%; the sulfonated product is hydrolyzed with 20% KOH solution at 135° C. for 2 hours to obtain potassium benzenesulfonate of TIB.

[0038] Adsorbent preparation: The preparation process of the carrier is the same as in Example 1, and the porogen is changed to potassium benzenesulfonate of TIB. The molar ratio of potassium benzenesulfonate of TIB to aluminum isopropoxide is 0.045:1, and the average particle size is ob...

Embodiment 3

[0044] Preparation of porogen: TIB is mixed with synthesis gas (CO:H 2 =1:1) reaction, with 0.01wt% rhodium octanoate as catalyst, after reaction time 20h at temperature 150°C and pressure 15MPa, then switch the synthesis gas to hydrogen, hydrogenation at 150°C and 15MPa for 5h to obtain iso-containing A mixture of tridecyl alcohol and isomeric dodecane, and the isomeric dodecane is removed by rectification to obtain isotridecyl alcohol. In the reaction kettle, the isotridecyl alcohol prepared by TIB is used as the initiator, and 0.2% KOH is used as the catalyst to react with ethylene oxide whose molar mass is 3 times that of the isotridecyl alcohol at 0.5 MPa and 85°C. 5h, then aged at 120°C for 1 hour and then cooled to obtain isomeric tridecyl alcohol polyoxyethyl ether with an ethylene oxide addition number of 3.

[0045] Adsorbent preparation: the preparation process of the carrier is the same as in Example 1, and the porogen is changed to isomeric tridecyl alcohol polyo...

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Abstract

The present invention relates to a method for preparing odorless isododecane. The isobutene trimer (TIB) reacts with hydrogen in the hydrogenation reactor to prepare crude isododecane, which is dehydrated and dried, and then enters the first-stage deodorization adsorption tower and protects the deodorization tower to obtain the finished product. Structure dodecane. The first-stage deodorization tower can be switched in parallel. The deodorization adsorbent adopts a dual-function adsorbent with adsorption-hydrogenation reduction. The regeneration desorption adopts the method of hydrogenation reduction. The regeneration temperature is low, the life of the adsorbent is long, and the requirements for equipment materials are low. , No need to use hot nitrogen or steam to purge and replace before regeneration, low energy consumption, no oxygen for regeneration, no danger of combustion and explosion, and basically no loss of effective materials adsorbed in the adsorbent. Effectively solve the contradictions among factors such as three wastes, energy consumption, material consumption, materials and safety.

Description

technical field [0001] The invention relates to a method for preparing odorless isododecane, in particular to a method for preparing odorless isododecane by hydrogenating and deodorizing isobutene trimers. Background technique [0002] Isododecane is a highly branched saturated dodecane, which does not have the oily smell of low-carbon alkanes, and has a relatively fast volatilization speed. It can be used as a substitute for volatile silicone oil for The skin feels very refreshing when used in cosmetics, and can be widely used in various cosmetics, skin care / hair care products, aerosols and other fields. [0003] Isododecane usually comes from the hydrogenation of isobutylene terpolymer (TIB), but the hydrogenation products generally have a certain odor. Patent CN200480006931 believes that the odor-generating substances are trace oxygen-containing substances generated by the contact reaction between oligoolefins and oxygen. Aldehydes, alcohols, esters and other impurities....

Claims

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Application Information

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IPC IPC(8): C07C9/16C07C5/03C07C7/12B01J20/28B01D53/02
CPCB01D53/02B01J20/28014B01J20/28061B01J20/2808B01J20/28083C07C5/03C07C7/005C07C7/12C07C2523/72C07C9/16
Inventor 袁帅黄少峰王中华董龙跃刘振峰吕艳红姜庆梅黎源
Owner WANHUA CHEM GRP CO LTD
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