CN104592345A

CN104592345A - Method for extracting tigogenin from sisal pulp

Info

Publication number: CN104592345A
Application number: CN201510055402.6A
Authority: CN
Inventors: 潘增强
Original assignee: Individual
Current assignee: Individual
Priority date: 2015-02-04
Filing date: 2015-02-04
Publication date: 2015-05-06

Abstract

The invention discloses a method for extracting tigogenin from sisal pulp. The method is characterized by comprising the following steps: 1. thickening sisal pulp: storing prepared back sisal pulp in a storage pool for natural precipitation, and pumping out supernatant to obtain thickened sisal pulp; 2. acid blending: pumping the sisal pulp into an acid blending tank, and quantitatively adding concentrated sulfuric acid and oxalic acid while stirring; 3. carrying out a hydrolysis reaction: pumping the sisal pulp blended with acid into a reaction kettle, heating to hydrolyze the sisal pulp, filter pressing by a press filter after discharging, carrying out environmental protection treatment on filtrate taken as wastewater, and drying filter residues in the sun or by a stove to obtain hydrolysate; 4. drying the hydrolysate: drying the hydrolysate in the sun or by a stove; 5. separating impurities: crushing the hydrolysate, putting the crushed hydrolysate in a reaction vessel, adding alcohol and heating, filter pressing by the press filter after discharging, concentrating the filtrate to recycle alcohol, wherein residual viscous condensates left after concentration are impurities; scooping up the residual viscous condensates to serve as wastes, and collecting the filter residues for later use; 6. calcifying the filter residues: mixing the filter residues with pulverized lime to have a calcification reaction to obtain a calcium compound; 7. saponin extracting and decoloring: putting the calcium compound in the reaction vessel, adding alcohol and activated carbon, heating, filter pressing by the press filter after discharging, removing the filter residues, concentrating the filtrate to recycle alcohol to 50%, discharging the concentrated solution to a storage tank, naturally cooling for 24 hours to crystallize the concentrated solution, filtering the crystals, concentrating the mother liquor to 1/3, discharging the concentrated solution to the storage tank, cooling for 24 hours to crystallize the concentrated solution, mixing the filtered crystals and the above crystals and drying to obtain a tigogenin product.

Description

A kind of by sisal hemp pulp extraction tigogenin method

Technical field

The invention discloses a kind of by sisal hemp pulp extraction tigogenin method, is by sisal hemp pulp extracting directly tigogenin method.

Background technology

Traditional tigogenin extracting method:

1, sisal hemp sheet takes out flax silk through mechanical scutching, and remaining tankage one dregs of linseeds or sesame seeds extrude juice through machinery again and enter storage pond, and juice is natural sedimentation in pond, pumps supernatant liquid, and the material of bottom thickness is called jute pulp;

2, jute pulp pump is extracted into threshing ground and naturally dries, and obtains numb cream;

3, load reactor after numb cream fragmentation, add dilute sulphuric acid and heat the reaction that is hydrolyzed, obtaining hydrolyzate;

4, after hydrolyzate discharging through pressure filter dehydration, filtrate goes environmental protection treatment as waste water, and filter residue and milk of lime mix and carries out calcify reaction and obtain calcified material;

5, load extractor after calcified material drying, add alcohol and heating is extracted through Filter Press after discharging, filter residue discards, and obtains saponin mixed solution;

6, filtrate is again through activated carbon decolorizing, then elimination gac, and filtrate concentrates, and concentrated solution is discharged in basin, leaves standstill 24 hours spontaneous nucleations obtain crystallization saponin in indoor;

7, crystal solution suction filtration obtains tigogenin xln, mother liquor concentrations recovered alcohol to three/mono-, concentrated solution is discharged in basin, 24 hours spontaneous nucleations are left standstill in indoor, refilter and obtain saponin xln, two kinds of xln merge oven dry and obtain tigogenin product, and remaining mother liquor reconcentration recovered alcohol, to dry, shovels out impurity as waste material.

Naturally the shortcoming of numb cream is dried:

1, jute pulp moisture more than 93%, viscosity is large, and the time of naturally drying is long;

2, ted jute pulp and need big area threshing ground, build threshing ground land occupation;

3, ted numb cream and throw work launch-work, labour intensity is large;

4, be difficult to rainy season dry, impact is produced.

Summary of the invention

The present invention replaces numb cream extracting directly tigogenin with jute pulp, saves and dries jute pulp operation.

Jute pulp extracting directly tigogenin, mainly through following steps:

1, jute pulp enrichment:

Still higher from the jute pulp moisture content that retracts of processing family, the natural sedimentation 48 hours again of storage pond need be put into, take supernatant liquid away and obtain enrichment jute pulp.

2, complex acid:

Jute pulp is extracted into complex acid groove, under agitation quantitatively adds the vitriol oil and oxalic acid.

3, hydrolysis reaction:

Jute pulp after complex acid is evacuated to reactor, and heating makes it be hydrolyzed, and through pressure filter press filtration after discharging, filtrate goes environmental protection treatment as waste water, obtains hydrolyzate.

4, hydrolyzate is dry:

Hydrolyzate dries or dries,

5, separating impurity:

Load reactor after hydrolyzate fragmentation, add alcohol and heat, through pressure filter press filtration after discharging, filtrate concentration and recovery alcohol, thickness cured article remaining after concentrated is impurity, and scoop up as waste material, filter residue is stand-by.

6, filter residue calcification:

Filter residue and lime powder mixing calcify reaction, obtain calcified material.

7, saponin is extracted and decolouring:

Calcified material loads reactor, add alcohol and gac and heat, through pressure filter press filtration after discharging, filter residue discards, filtrate concentration and recovery alcohol to 50%, concentrated solution blowing is to storage tank, naturally cooling 24 is little leaches crystallisate up to its crystallization, and mother liquor is concentrated into 1/3rd again, concentrated solution blowing cools 24 little of its crystallization to storage tank, the crystallization leached and above-mentioned crystallization merge oven dry and obtain tigogenin product.

Present invention process jute pulp extracting directly tigogenin, is characterized in that:

1, the every m3 jute pulp of described step 2 joins 82 kilograms, sulfuric acid, oxalic acid 0.5 kilogram;

2, the hydrolysis temperature of described step 3 was 105 DEG C, this temperature 4 hours;

3, described sulfuric acid concentration 95%, oxalic acid quality 99%;

4, described step 5,7 alcoholic extraction temperature be alcohol boiling temperature > 79 DEG C;

5, described gac model is 783 types;

6, described ethanol concn 95%, the add-on of alcoholic extraction impurity is hydrolyzate 6 times of volume weights, and the add-on of alcoholic extraction saponin is calcified material 6 times of volume weights;

7, described step 6 filter residue and lime powder blending ratio are 100: 9.

The advantage of the technology of the present invention is:

1, because jute pulp is with adstringency, be difficult to remove with dilute sulphuric acid separately during hydrolysis, affect quality product, oxalic acid can remove adstringency in jute pulp, thus adds a small amount of oxalic acid when being hydrolyzed and removes adstringency, ensure quality product;

2, jute pulp extracting directly tigogenin, jute pulp is per ton after giving money as a gift uses manpower and material resources sparingly 1000 yuan at a discount;

3, without threshing ground, economize the land resource;

4, normally produce rainy season in the same old way, do not affect output.

Embodiment

Sisal hemp pulp extracts tigogenin method, and be exactly realization sisal hemp pulp extracting directly tigogenin, implementation step is:

1, jute pulp enrichment:

2, system hydrolysis:

From storage pond, jute pulp is taken out to reactor with pump, adding 82 kilograms of concentration by every m3 jute pulp is 95% sulfuric acid, be the oxalic acid of 99% with 0.5 kilogram of quality, load onto thermometer, heat to 105 DEG C, react hydrolysis 4 hours at this temperature, discharging when temperature drops to about 70 DEG C, after Filter Press, filtrate does wastewater treatment, filter cake through pulverizer broken hydrolyzate.

3, hydrolyzate is dry:

Hydrolyzate Tumblies Dry or naturally dries.

4, separating impurity:

Dried to above-mentioned (3) hydrolyzate fragmentation is loaded in reactor on the about 20th, add the volume of hydrolyzate 6 times, concentration is the alcohol of 95%, loads onto agitator and thermometer, heats and stirs, keep alcohol boiling temperature 1 hour, treat that temperature drops to about 60 DEG C, then discharging and filtering, filtrate evaporation recovered alcohol, evaporate to dryness alcohol is left thickness solid fraction impurity and scoops up and discard, and filter residue is stand-by.

5, filter residue calcification:

Above-mentioned filter residue is added lime powder 9 jin mixing by every 100 jin, and calcify reaction 30 minutes, obtains calcified material.

6, saponin and decolouring is extracted:

Above-mentioned (5) calcified material is loaded in reactor, add 6% volume of calcified material weight, model is that 783 type gacs are for decolouring, add calcified material weight 6 times of volumes again, concentration 95% alcohol, load onto agitator and thermometer, heat and stir, keep alcohol boiling temperature 1 hour, treat that temperature drops to about 60 DEG C, then discharging and filtering, filter residue discards, filtrate evaporation recovered alcohol to 50%, concentrated solution blowing is to storage tank, naturally cooling 24 is little of its crystallization, leach crystallisate, mother liquor is concentrated into 1/3rd again, concentrated solution blowing cools 24 little of its crystallization to storage tank, the crystallization leached and above-mentioned crystallization merge oven dry and obtain tigogenin product.

Claims

1. extract a tigogenin method by sisal hemp pulp, it is characterized in that comprising following step gathers:

(1) jute pulp enrichment:

Jute pulp puts into storage pond natural sedimentation again, takes supernatant liquid away and obtains enrichment jute pulp.

(2) complex acid:

(3) reaction hydrolysis:

Jute pulp after complex acid is evacuated to reactor, and heating makes it be hydrolyzed, and through pressure filter press filtration after discharging, filtrate goes environmental protection treatment as waste water, and filter residue dries or dries, and obtains hydrolyzate.

(4) hydrolyzate is dry:

Hydrolyzate is dried or is dried.

(5) separating impurity:

(6) filter residue calcification:

(7) saponin is extracted and decolouring:

2. extract tigogenin method by sisal hemp pulp according to claim 1, it is characterized in that:

Described jute pulp water content > 70%.