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 Process for extracting lignin from lignocellulosic material using an aqueous organic solvent and an acid neutralizing agent

Details
Inventors: Roberts, Ronnie S.; Muzzy, John D.; Faass, George S.;
Assignee: Georgia Tech Research Corp. (Atlanta, GA)
Primary Examiner: Alvo; Steve
Assistant Examiner:
Attorney, Agent or Firm: Newton, Hopkins & Ormsby

A process for the delignification of cellulosic materials, wherein a high-yield cellulose pulp and high-value by-product, such as reactive lignins of low molecular weight are produced, which comprises degassing lignocellulosic material, rapidly heating the lignocellulosic material in a liquor comprising water, an organic solvent and a buffer thereby maintaining a substantially neutral solvent extraction, such that said lignocellulosic material is cooked in the liquor as it is heated from a temperature of 150.degree. C. to a selected maximum temperature in the range of 200.degree. to 280.degree. C.; and rapidly cooling the mixture to a temperature less than 150.degree. C. The reaction is controlled to maximize reactive lignin solvation while suppressing cellulose degradation.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS With reference to FIG.
1, the results shown therein were in relation to a series of cooks in which the mixture of wood material and liquor was heated rapidly to a maximum temperature in the range of from 100.
degree.
C.
to 280.
degree.
C.
and then immediately cooled very rapidly.
As will be recognized, such cooking omits the third stage of cooking.
The lignocellulosic material was tulip popular chips which were reduced to a nominal 1 mm particulate size by Wiley milling.
Pulping cooks were performed using a 650 ml stirred batch reactor manufactured by Pharr Instruments, Inc.
The material was first degassed followed by soaking in a pulping liquor composed of ethanol, water, sodium bicarbonate and methylanthraquinone in proportions as follows: Ethanol--180 ml Water--120 ml Sodium bicarbonate--7.
7 g Wood (dry)--33 g MAQ--1.
2 g The mixture of liquor and material submerged therein was charged into the reactor, rapidly heated to the desired temperature and immediately cooled rapidly.
The results of such cooks are shown in FIG.
1 wherein it will be seen that delignification essentially does not occur until the temperature exceeds about 160.
degree.
C.
, but thereafter proceeds quite rapidly.
The residual lignin content of the pulp does not follow the delignification curve except as to general trend.
In these cooks, which are identified as nonisothermal cooks for convenience, the maximum time taken to heat to temperature was about 32 minutes and the maximum time taken for cooling was about 12 minutes.
A further series of cooks was undertaken, these being named for convenience as isothermal cooks.
In these isothermal cooks, the reactor was heated to a specific temperature of from 200.
degree.
C.
to 260.
degree.
C.
, held at that temperature for up to 45 minutes and then rapidly cooled.
As will be apparent, the so called isothermal cooks are of the type which include the third stage of cooking in accord with this invention.
A comparison between the isothermal and the nonisothermal cooks is shown in FIG



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