A kind of two-stage leaches the method for gutta-percha
Technical field
The present invention relates to a kind of extracting method of gutta-percha, specifically refer to that utilizing freezing of gutta-percha to analyse filtered liquid carries out first step leaching, evaporation condensate carries out the processing method of second stage leaching.
Background technology
The swollen glue of Du, is called gutta-percha or Ba Lata (Balata) in the world, is the isomers of natural para rubber, is using trans-polyisoprene.Gutta-percha can, as medical material, rubber item etc., can also make intermingling material with other material blend by sulfuration and modification, and application prospect is very wide.
The extracting method of gutta-percha has reflux extraction, Continuous Countercurrent Extraction method, soxhlet extraction method etc., existing extracting method has been obtained compared with quantum jump on extraction yield, but cannot solve all the time due to the expensive problem causing that solvent-oil ratio is large, energy consumption is high, become the technology barriers that hinder gutta-percha industrialized implementation.
The molten consumption of existing Gutta extraction technology reason high, that energy consumption is high is: after adopting the non-polar solvents such as sherwood oil to extract, need to gutta-percha be separated out to separation by freezing to analyse, freeze and analyse mother liquor and just recycle after whole evaporative condensers, in evaporative condenser process owing to relating to phase transformation, thereby need to consume higher energy, also can increase solvent loss.
Therefore, exploitation less energy-consumption, low molten consumption, can ensure that again gutta-percha has the Gutta extraction technology of higher extracted rate, significant for the development of bark of eucommia industry.
Summary of the invention
The problem existing for solving Gutta extraction prior art, the inventor, through lot of experiments, invents a kind of method of two-stage leaching gutta-percha finally, use the method to extract gutta-percha, higher extraction yield can be ensured, energy consumption and molten consumption can be significantly reduced again, cost-saving.
The present invention is from the ratio additional issue of gutta-percha leach liquor concentrates, and its technical scheme is:
(1) the ratio evaporation concentration of gutta-percha leach liquor: by the solvent evaporation 40-60% in the sherwood oil gutta-percha leach liquor of 60-90 DEG C of boiling range, the solvent condenses after evaporation is for subsequent use, and evaporation concentration liquid freezes and is separated by decantation to gutta-percha at 0-5 DEG C, for subsequent use after filtering.
(2) first step is extracted: analyse mother liquor as solvent to freeze, material is carried out to first step counterflow leaching at 40-50 DEG C, can auxiliary ultrasonic in leaching process and stir, and utilize hyperacoustic cavitation effect to strengthen the stripping of gutta-percha.Owing to easily hardening in Gutta extraction process, hinder mass transfer, stirring and ultrasonic wave can also effectively prevent that material from hardening.
(3) extract the second stage: the material after with the solvent after evaporative condenser, the first step being extracted carries out second stage counterflow leaching at 40-50 DEG C, also can auxiliary ultrasonic in leaching process and stir, and utilize hyperacoustic cavitation effect to strengthen the stripping of gutta-percha.Owing to easily hardening in Gutta extraction process, hinder mass transfer, stirring and ultrasonic wave can also effectively prevent that material from hardening.
(4) leach liquor that combining step (2) and step (3) obtain returns to step (1) and carries out ratio evaporation concentration.
Utilize aforesaid method to extract gutta-percha, in material, the residual rate of gutta-percha is stabilized in below 0.5%, equally matched with soxhlet extraction, and energy consumption and molten consumption decline respectively 15-30% and 10-20% have very strong practical value.
Compared with prior art, the invention has the beneficial effects as follows:
Employing two-stage countercurrent leaches, and the full adverse current segmentation of gutta-percha in material is leached, and under the cooperation of ultrasonic wave and stirring, has strengthened dissolving and the mass transfer of gutta-percha, has prevented that effectively the material in continuous leaching process from hardening.
First start to carry out ratio evaporation concentration from leach liquor, and determined evaporation ratio by great many of experiments, not only save energy, reduce solvent loss but also guarantee the quality of gutta-percha.
Carry out ratio evaporation instead of solvent pervaporation, energy steam saving, also can reduce solvent loss, avoids the ether solubility impurity that evaporation brings to be detained in glue simultaneously, causes impurity in glue to exceed standard, and affects quality; Can cause again ether solubility impurity in solvent to get more and more but do not carry out evaporation concentration, the solubility property of solvent declines, although can be energy-conservation, can significantly reduce the extraction yield of gutta-percha.
The first step leaches owing to being undrawn material, thereby mass transfer power is larger, adopts to freeze to analyse mother liquor and also can guarantee higher extraction yield; After the solvent condenses of evaporation, carry out second stage material leaching, can increase mass transfer power, strengthen the stripping of gutta-percha, make the gutta-percha residual quantity in material minimum.
Embodiment
Below the method that leaches gutta-percha from two-stage is elaborated.
Embodiment 1:
(1) the ratio evaporation concentration of gutta-percha leach liquor: by the solvent evaporation 42% in the sherwood oil gutta-percha leach liquor of 60-90 DEG C of boiling range, the solvent condenses after evaporation is for subsequent use, and evaporation concentration liquid freezes and is separated by decantation to gutta-percha at 1 DEG C, for subsequent use after filtering.
(2) first step is extracted: analyse mother liquor as solvent to freeze, material is carried out to first step counterflow leaching at 48 DEG C, auxiliary ultrasonic and stirring in leaching process.
(3) extract the second stage: the material after with the solvent after evaporative condenser, the first step being extracted carries out second stage counterflow leaching at 43 DEG C, auxiliary ultrasonic and stirring in leaching process.
(4) leach liquor that combining step (2) and step (3) obtain returns to step (1) and carries out ratio evaporation concentration.
Utilize aforesaid method to extract gutta-percha, in material, the residual rate of gutta-percha is 0.41%, equally matched with soxhlet extraction, and energy consumption and molten consumption decline respectively 26% and 17%, have very strong practical value.
Embodiment 2
(1) the ratio evaporation concentration of gutta-percha leach liquor: by the solvent evaporation 57% in the sherwood oil gutta-percha leach liquor of 60-90 DEG C of boiling range, the solvent condenses after evaporation is for subsequent use, and evaporation concentration liquid freezes and is separated by decantation to gutta-percha at 4 DEG C, for subsequent use after filtering.
(2) first step is extracted: analyse mother liquor as solvent to freeze, material is carried out to first step counterflow leaching at 42 DEG C, auxiliary ultrasonic and stirring in leaching process.
(3) extract the second stage: the material after with the solvent after evaporative condenser, the first step being extracted carries out second stage counterflow leaching at 47 DEG C, auxiliary ultrasonic and stirring in leaching process.
(4) leach liquor that combining step (2) and step (3) obtain returns to step (1) and carries out ratio evaporation concentration.
Utilize aforesaid method to extract gutta-percha, in material, the residual rate of gutta-percha is 0.45%, equally matched with soxhlet extraction, and energy consumption and molten consumption decline respectively 18% and 13%, have very strong practical value.