CN108948375A - A kind of preparation method of filament gutta-percha - Google Patents

Abstract

The present invention relates to a kind of preparation method of filament gutta-percha, following steps: 1) adding sodium hydroxide solution into the folium cortex eucommiae after coarse crushing, in oscillation treatment, removes the cuticula in folium cortex eucommiae；2) weigh thick enzyme powder, buffer solution be added, 50 DEG C stirred in water bath 45 minutes, filtered with absorbent cotton, it is stored refrigerated stand-by after sealing；3) removed after alkali process into step 1 be added in the filter residue blade of cuticula cellulase solution and and enzymolysis liquid, shaken 2-4 hours at 50 DEG C and under the conditions of 120r/min；4) petroleum ether will be added in the Eucommia ulmoides Oliv. leaves after alkali and enzymatic treatment, refluxing extraction 2 hours at 85 DEG C are cooled to room temperature after filtering while hot, freeze at 0 DEG C and refilter to obtain gutta-percha after forty minutes.The method of the invention is extracted with petroleum ether using after alkali removal cuticula by enzymolysis processing folium cortex eucommiae again, is had preferable changing effect, is a kind of high conversion rate; the high preparation method of product quality; and short preparation period, it is at low cost, it is suitable for scale production.

Description

A kind of preparation method of filament gutta-percha

Technical field

The invention belongs to effective ingredients in plant to extract field, and in particular to the preparation side of filament gutta-percha in a kind of folium cortex eucommiae Method.

Background technique

Gutta-percha is commonly called as gutta-percha or balata, is the native biopolymer material contained in Cortex Eucommiae plant, Have the function of many unique properties and.Currently, most research is concentrated mainly on raising in the extraction research of gutta-percha In the target of Gutta extraction amount, however, the extraction of gutta-percha is not only recovery rate one side, it should also be taken into account that being had The product of good physical behavior.In existing Gutta extraction document and patent, the overwhelming majority is required Bark of Eucommia Ulmoides and Du Zhong Ye is crushed, and dissolution efficiency of the gutta-percha in Extraction solvent can be improved in such processing, but Folium glue wire is outside machinery It is destroyed to a certain extent under the action of power, this shows that the preprocess method of raw material largely determines extracted Du The properties such as the elasticity of secondary glue and wilful and tensile strength.Natural gutta-percha high molecular polymer be under the action of enzyme and at, It is different with artificial synthesized high molecular polymer, catalyst and oligopolymer substance without containing small molecule, in the item of high polymerization degree Under part, the even more rich unique rubber and plastic dual character of gutta-percha.

Summary of the invention

Technical problem to be solved by the invention is to provide Bark of Eucommia Ulmoides and folium cortex eucommiae are first removed cuticula then to digest again The method that solvent extraction prepares filament gutta-percha is carried out, this method is easy, only uses a small amount of lye and enzymatic hydrolysis solution, preparation week Phase is short, at low cost, meets the requirement of green and safety, and tensile strength, elongation at break, tearing are strong in resulting filament gutta-percha Degree is significantly stronger than the gutta-percha prepared after tradition machinery is crushed, suitable for scale production.

Present invention provide the technical scheme that a kind of preparation method of filament gutta-percha, includes the following steps:

(1) sodium hydroxide solution that ph is 11, oscillation treatment 6 hours, mistake at 30-70 DEG C are added into the folium cortex eucommiae after coarse crushing Filter removes the cuticula in folium cortex eucommiae；

(2) weigh thick enzyme powder 5g, the buffer solution 200ml that PH is 4 be added, 50 DEG C stirred in water bath 45 minutes, use absorbent cotton Filtering, it is stored refrigerated stand-by after enzymolysis liquid obtained is sealed；The thick enzyme powder is β -1,4 glycosidic bond or glucan or glucan Hydrolase；Buffer solution mixed solution made of Citric Acid Mono and sodium bicarbonate, in mass ratio, Citric Acid Mono: Sodium bicarbonate=6:4；

(3) into step 1 after alkali process remove cuticula Eucommia ulmoides Oliv. leaves in be added 50mlPH be 4 cellulase solution and The enzymolysis liquid that 100ml PH is 4 shakes 2-4 hours under the conditions of 50 DEG C and 120r/min；

(4) 120ml petroleum ether is added in the Eucommia ulmoides Oliv. leaves by 50g after alkali and enzymatic treatment, refluxing extraction 2 is small at 85 DEG C When, while hot with being cooled to room temperature after conventional filter paper or 200 mesh filter-cloth filterings, is freezed at 0 DEG C and refilter to obtain Du after forty minutes Secondary glue.

The method of the present invention for preparing filament gutta-percha digests folium cortex eucommiae after removing cuticula using alkali, Then it is extracting, is solving the problems, such as that the broken obtained gutta-percha intensity of tradition machinery is inadequate.

The invention has the following advantages:

The method of the present invention is combined zymolysis technique using the renewable skin of Cortex Eucommiae of growing up and leaf object as raw material, by removing cuticula, enzymatic hydrolysis Raw material optimizes product preparation process process；Tensile strength, elongation at break and tearing strength can be improved in product；Side of the present invention Method is easy, and short preparation period is at low cost, meets the requirement of environmental protection and safety, suitable for scale production.

Specific embodiment

The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..Heretofore described Bark of Eucommia Ulmoides And folium cortex eucommiae is purchased from Hubei Yun Hao pharmaceutcal corporation, Ltd, thick enzyme powder is purchased from Zhangjagang City Jin Yuan biochemical industry Co., Ltd, buffering Solution is to provide for oneself.

Embodiment 1

(1) folium cortex eucommiae is processed into the blade that diameter is 1-3cm, is placed in 250ml conical beaker, and addition concentration is 1%-5%(W/V) Sodium hydroxide solution 200ml, vibrate 6 hours, filter on 30-70 DEG C, the shaking table of 120r/min, remove the angle in folium cortex eucommiae Matter layer；To will remove the Eucommia ulmoides Oliv. leaves of destratum corneum with distilled water flushing to PH be it is neutral, then drying to constant weight；

(2) weigh thick enzyme powder 5g, the buffer solution 200ml that PH is 4 be added, 50 DEG C stirred in water bath 45 minutes, use absorbent cotton Filtering, enzymolysis liquid obtained are sealed in triangular flask and are put into stored refrigerated stand-by in refrigerator；

(3) into step 1 through alkali process except be added in the Eucommia ulmoides Oliv. leaves after destratum corneum cellulase solution that 50mlPH is 4 and The enzymolysis liquid that 100ml PH is 4, is placed in 50 DEG C of water-bath, and shaking is filtered after 2-4 hours under the conditions of revolving speed is 120r/min； Drying to constant weight at 50 DEG C for treated Eucommia ulmoides Oliv. leaves；

(4) 120ml petroleum ether is added in the Eucommia ulmoides Oliv. leaves by 50g after alkali and enzymatic treatment, the reflux extraction 2 under the conditions of 85 DEG C Hour, while hot with petroleum ether solution containing glue is obtained after conventional filter paper or 200 mesh filter-cloth filterings, it is cooled to room temperature, at 0 DEG C Freezing refilters to obtain gutta-percha after forty minutes；

By gutta-percha that step 4 obtains in requiring to be paved into lengthy motion picture according to measurement on polyfluortetraethylene plate before unseasoned, now It is evaporated completely petroleum ether solvent under room temperature, makes its melting adhered integral in 80 DEG C of baking ovens.Tensile strength, elongation at break and Tearing strength on the computer-controlled electronic universal tester of WDW-10C type (Hualong Detector Co., Ltd., Shanghai) measures (measurement result are as follows: tensile strength 60.5MPa, elongation at break 24%, tearing strength 36KN/M) shows the gutta-percha tool There is good physical property.

Embodiment 2

(1) folium cortex eucommiae is processed into the blade that diameter is 1-3cm, is placed in 250ml conical beaker, and addition concentration is 1%-5%(W/V) Sodium hydroxide solution 200ml, vibrate 6 hours, filter on 30-70 DEG C, the shaking table of 120r/min, remove the angle in folium cortex eucommiae Matter layer；To will remove the Eucommia ulmoides Oliv. leaves of destratum corneum with distilled water flushing to PH be it is neutral, then drying to constant weight；

(2) weigh thick enzyme powder 5g, the buffer solution 200ml that PH is 4 be added, 50 DEG C stirred in water bath 45 minutes, use absorbent cotton Filtering, enzymolysis liquid obtained are sealed in triangular flask and are put into stored refrigerated stand-by in refrigerator；

(3) into step 1 through alkali process except be added in the Eucommia ulmoides Oliv. leaves after destratum corneum cellulase solution that 50mlPH is 4 and The enzymolysis liquid that 100ml PH is 4, is placed in 50 DEG C of water-bath, and shaking is filtered after 2-4 hours under the conditions of revolving speed is 120r/min； Drying to constant weight at 50 DEG C for treated Eucommia ulmoides Oliv. leaves；

(4) 120ml petroleum ether is added in the Eucommia ulmoides Oliv. leaves by 50g after alkali and enzymatic treatment, the reflux extraction 2 under the conditions of 85 DEG C Hour, while hot with petroleum ether solution containing glue is obtained after conventional filter paper or 200 mesh filter-cloth filterings, it is cooled to room temperature, at 0 DEG C Freezing refilters to obtain gutta-percha after forty minutes；

By gutta-percha that step 4 obtains in requiring to be paved into lengthy motion picture according to measurement on polyfluortetraethylene plate before unseasoned, now It is evaporated completely petroleum ether solvent under room temperature, makes its melting adhered integral in 80 DEG C of baking ovens.Tensile strength, elongation at break and Tearing strength on the computer-controlled electronic universal tester of WDW-10C type (Hualong Detector Co., Ltd., Shanghai) measures (measurement result are as follows: tensile strength 59.8MPa, elongation at break 23.2%, tearing strength 37.1KN/M) shows the Cortex Eucommiae Glue has good physical property.

Claims (1)

1. a kind of preparation method of filament gutta-percha, which comprises the steps of:

(1) sodium hydroxide solution that ph is 11, oscillation treatment 6 hours, mistake at 30-70 DEG C are added into the folium cortex eucommiae after coarse crushing Filter removes the cuticula in folium cortex eucommiae；

(2) weigh thick enzyme powder 5g, the buffer solution 200ml that PH is 4 be added, 50 DEG C stirred in water bath 45 minutes, use absorbent cotton Filtering, it is stored refrigerated stand-by after enzymolysis liquid obtained is sealed；The thick enzyme powder is β -1,4 glycosidic bond or glucan or glucan Hydrolase；Buffer solution mixed solution made of Citric Acid Mono and sodium bicarbonate, in mass ratio, Citric Acid Mono: Sodium bicarbonate=6:4；

(3) into step 1 after alkali process remove cuticula Eucommia ulmoides Oliv. leaves in be added 50mlPH be 4 cellulase solution and The enzymolysis liquid that 100ml PH is 4 shakes 2-4 hours under the conditions of 50 DEG C and 120r/min；

(4) 120ml petroleum ether is added in the Eucommia ulmoides Oliv. leaves by 50g after alkali and enzymatic treatment, refluxing extraction 2 is small at 85 DEG C When, while hot with being cooled to room temperature after conventional filter paper or 200 mesh filter-cloth filterings, is freezed at 0 DEG C and refilter to obtain Du after forty minutes Secondary glue.