CN108783554A - A kind of leakage of efficient anti-seepage carries capsule with diuresis promoting function and preparation method thereof - Google Patents

A kind of leakage of efficient anti-seepage carries capsule with diuresis promoting function and preparation method thereof Download PDF

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Publication number
CN108783554A
CN108783554A CN201810684856.3A CN201810684856A CN108783554A CN 108783554 A CN108783554 A CN 108783554A CN 201810684856 A CN201810684856 A CN 201810684856A CN 108783554 A CN108783554 A CN 108783554A
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CN
China
Prior art keywords
capsule
layer
water
water blocking
blocking layer
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Withdrawn
Application number
CN201810684856.3A
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Chinese (zh)
Inventor
赵瑾朝
黄乐平
黄伟
郭庆
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Wuhan Textile University
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Wuhan Textile University
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Priority to CN201810684856.3A priority Critical patent/CN108783554A/en
Publication of CN108783554A publication Critical patent/CN108783554A/en
Priority to CN201910552211.9A priority patent/CN110250549B/en
Withdrawn legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/015Inorganic compounds
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/03Organic compounds
    • A23L29/035Organic compounds containing oxygen as heteroatom
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/03Organic compounds
    • A23L29/045Organic compounds containing nitrogen as heteroatom
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P20/00Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/20Making of laminated, multi-layered, stuffed or hollow foodstuffs, e.g. by wrapping in preformed edible dough sheets or in edible food containers
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/12Steaming, curing, or flavouring tobacco
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4808Preparations in capsules, e.g. of gelatin, of chocolate characterised by the form of the capsule or the structure of the filling; Capsules containing small tablets; Capsules with outer layer for immediate drug release
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4816Wall or shell material
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The present invention relates to a kind of efficient anti-seepages to leak load capsule with diuresis promoting function and preparation method thereof, capsule is at least three-decker, it is followed successively by sandwich layer, cyst wall layer, water blocking layer from inside to outside, water blocking layer coats cyst wall layer, its material is polybutylcyanoacrylate, 7 days permeability rates that efficient anti-seepage leakage carries capsule with diuresis promoting function are less than 4%, sphericity SF<0.07, capsule prepared by this method, ratio of briquetting is high, and smooth in appearance is mellow and full, uniform particle diameter, and the impermeable effect that blocks water is remarkable, and Storage period is long, and manufacturing process is easy, can be directly used for food, medicine and cigarette products processing.

Description

A kind of leakage of efficient anti-seepage carries capsule with diuresis promoting function and preparation method thereof
Technical field
The invention belongs to capsule preparation fields, and in particular to a kind of efficient anti-seepage leakage load capsule with diuresis promoting function.
Background technology
Get up water or aqueous soluble active constituent environmental sealing to form capsule using encapsulation techniques, keeps moisture in capsule It is always the research hotspot and difficult point in the fields such as food, medicine, tobacco in transport phase and shelf life long-time storage ne-leakage.
The selection of capsule wall material determines the mechanical property and permeance property of capsule.Alginic acid calcium salt is food and glue,medicinal Most common wall material in capsule, using ionic calcium soln as coagulating bath, the calcium alginate gel prepared using dropping preparation method has put into industry Metaplasia produces and obtains commercialization and promotes.
The prior art is more to the calcium alginate gel report of cladding oil or oil-soluble active ingredient, and for carrying water seaweed The report of sour calcium capsule is less.
Existing patent of invention, Publication No. CN102108136B, disclose a kind of dripping pills of cigarette additive lapping and With the application of the dripping pill and dripping pill of its package, the dripping pill is specifically disclosed for cigarette field, capsule is made using positive drop method, it should Capsule includes two layers, and sandwich layer and wrapping layer, lapping is by sodium alginate:Glycerine:Water is with (1-8):(0.5-5):(85- 100) ratio mixing composition, then capsule is made with the calcium ion solidification in coagulating bath.However, during we repeat to test It was found that capsule-wall made from this method is very thin, do not have mechanical strength needed for follow-up industrial processes, practicability is poor.
Existing patent of invention, Publication No. CN103815541A disclose a kind of three layers of cigarette capsule with diuresis promoting function, and wherein internal layer is Water, gelatin, preservative and essence, middle layer are sodium alginate, water, preservative, and outer layer is beeswax, paraffin and Brazil is cured is made. The invention is in original calcium alginate gel outer layer covers blended wax, to preventing the moisture spilling in capsule from having certain effect, but The interface binding power of the mixing wax layer of hydrophilic calcium alginate cyst wall layer and oleophylic is poor, wraps up uneven, cracky, and mix Wax melting temperature is closed at 50 DEG C or so, is vulnerable to the influence of ambient temperature, state labile.These result in the invention capsule without Method long-time storage, easy to leak.
Existing patent publication No. is CN103815542A on the basis of foregoing invention patent, discloses a kind of four layers of cigarette water Capsule, that is, using sodium alginate as raw material, forms one layer of protection in the 4th layer of the external sheath of original three layers of cigarette capsule with diuresis promoting function Film reduces the rupture of wax.However being still the problem of interface cohesion force difference between sodium alginate and wax coat influences the capsule Infiltrative principal element leads to the third layer and the 4th layer of uneven, the cracky of package of four layers of capsule with diuresis promoting function, easily seeps water.
Existing publication number is that CN105361242A discloses a kind of quick-fried pearl of Mobyneb cigarette based on liquid hoodle And preparation method thereof, existing publication number is that CN106914196A discloses one kind based on liquid hoodle preparation load water microcapsules Method.Two patents are by elder generation in water drops surface coated by hydrophobic particle, then coat instant drying adhesive and light-cured resin successively Water blocking layer realizes the preparation for the antiseep capsule that blocks water.However from the point of view of the effect for repeating experiment, by simply impregnating or The method of coating coats water blocking layer, and capsule cyst membrane became uneven is even, seriously affects the appearance and block-water effect of capsule.
From the prior art, the technology of preparing scheme for currently existing the impermeable capsule that blocks water, is by capsule One layer of water blocking layer is arranged in outer layer, prevents water or the aqueous solution extravasation of capsule internal layer, extends the validity period of capsule, but the prior art Capsule shaping degree and block-water effect are unsatisfactory.
Invention content
For deficiency in the prior art, the purpose of the present invention is to provide a kind of efficient anti-seepage leak adhesive capsule and its preparation sides Method.It solves capsule sandwich layer water or aqueous solution in the prior art easily to permeate, block-water effect is undesirable and forming degree is undesirable Technical problem.
To achieve the goals above, it is leaked the present invention provides a kind of efficient anti-seepage and carries capsule with diuresis promoting function, it is characterised in that:Capsule is At least three-decker, is followed successively by sandwich layer, cyst wall layer, the first water blocking layer from inside to outside, and first water blocking layer is coated on cyst wall layer Outside, it is the polymerizate of one or more cyanoacrylate compounds, it is small that efficient anti-seepage leakage carries 7 days permeability rates of capsule with diuresis promoting function In 4%, sphericity SF<0.07.
It is alginate, cellulose derivative, gelatin, chitosan, poly- second that efficient anti-seepage leakage, which carries capsule with diuresis promoting function cyst wall layer material, It is one or more in glycol, polyvinyl alcohol.
It is water or load water component that efficient anti-seepage leakage, which carries capsule with diuresis promoting function sandwich layer,.
The alpha-cyanoacrylate ester structure is CH2=C (CN) COOR, wherein R are alkyl, aryl, the alkoxy of C1-16.
The cyanoacrylate is Methyl 2-cyanoacrylate, cyanacrylate, Tisuacryl, cyano third At least one of olefin(e) acid monooctyl ester;
The cyanoacrylate that the present invention uses can be simple reagent, can also be the examination containing cyanoacrylate Agent, as long as can reach the requirement that cyanoacrylate forms the first water blocking layer outside cyst wall layer, the present invention can select city The product containing cyanoacrylate sold, such as Instant cement 502 or Instant cement 508.
The present invention selects to use cyanoacrylate compound as the first water blocking layer, cyanoacrylate compound Structure be CH2=C (CN) COOR, wherein R are alkyl, aryl, the alkoxy of C1-16, due on a carbon atom of alkene It is connected to-CN and-COOR so that β carbon atoms have strong suction electrical on alkene, the weak substance of compatibility are encountered, such as water, ammonia Anionic polymerisation rapidly occurs for base, alcohol etc. so that double bond cloud density reduces, and generates the polymerisation of moment, liquid Adhesive moment becomes solid-state.It is ingenious when preparation blocks water impermeable capsule for inventing the characteristic using cyanoacrylate Using the substance as the first water blocking layer, acted on using cyanoacrylate and water micro on capsule layer so that cyano Acrylate carries out polymerizing curable on micro-capsule surface layer, forms the first water blocking layer, and then reach the impermeable effect that blocks water.Permeability rate is adopted It is tested with weight method, specifically randomly selects 50 capsules, weigh its weight at regular intervals, calculate its weight-loss ratio, And be averaged, as a result reflect the impermeable effect of capsule, i.e. permeability rate, capsule prepared by the present invention 7 days it is permeable Rate is less than 4%, preferably smaller than 3%, is further preferably no larger than 2%;30 days permeability rates are less than 8%, preferably smaller than 5%, into one Step preferably smaller than 3%.
Capsule further includes the 4th layer, and the 4th layer is the second water blocking layer, and the second water blocking layer is coated on outside the first water blocking layer, and second Water blocking layer is light-cured resin, and the first water blocking layer can be fixed in the second water blocking layer, and further decreases the saturating of capsule Water rate.
According to the practical application of capsule, different core materials can be added, sandwich layer can be water, or aqueous group Part.For a kind of solute containing metal ion, with cyst wall layer raw material, especially sodium alginate ion can occur for this kind of solute It exchanges, obtains the cyst wall layer with cross-linked structure, and the sandwich layer for effectively wrapping up water or aqueous components forms ball-type capsule structure.
In order to prepare the capsule of the present invention, preparation method of the invention includes the following steps:(1) glue is prepared by dropping preparation method Capsule, sandwich layer are water or aqueous components, and cyst wall layer is alginate, cellulose derivative, gelatin, chitosan, polyethylene glycol, poly- second It is one or more in enol;(2) capsule surface coats the first water blocking layer;(3) the efficient anti-seepage leakage being prepared in step (2) Aqueous capsule surface coats the second water blocking layer.
Efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, which is characterized in that the dropping preparation method is anti-drop method, when preparing capsule Temperature be 50-80 DEG C.
Positive drop method and anti-drop method can prepare capsule, and positive drop method is that cyst material and core material are passed through coaxial double needle Dropping feeder is added drop-wise in solidification solution, the positive capsule for dripping method and preparing, and the cross-linking reaction of cyst wall layer is from outer wall to sandwich layer side To diffusion process.Anti- drop rule is that the sandwich layer solution for containing coagulating component is added drop-wise in cyst wall layer raw material, the anti-glue for dripping method and preparing Capsule, the cross-linking reaction of cyst wall are sandwich layers to cyst wall layer diffusion process.Positive drop method is different with the anti-dropwise addition sequence of drop method, makes cyst wall The curing degree of layer generates difference, and the capsule prepared using anti-drop method, size is easier to control, and wall thickness is big, Neng Goufang The exudation of sealing point can also meet the requirement that following process in the process crushes capsule intensity.The capsule prepared with anti-drop method is straight Diameter is 3+2mm.
Efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, which is characterized in that the method for the first water blocking layer of cladding is, by step (1) in a solvent, the solvent and water are immiscible, and do not react with cyanoacrylate, and solvent is for gained capsules disperse One or more of dimethyl carbonate, butyl acetate, chloroform, silicone oil, petroleum ether, toluene, n-hexane, atoleine, Cyanoacrylate compound is added dropwise to above-mentioned dispersion, until capsule surface forms the first water blocking layer.
The selected solvent of step (1) of the present invention be dimethyl carbonate, butyl acetate, chloroform, silicone oil, petroleum ether, One or more of toluene, n-hexane, atoleine, above-mentioned organic solvent and water are immiscible, not with cyanoacrylate Class compound reacts.The capsule prepared by step (1), cyst wall main component are calcium alginate hydrogel, surface Cyanoacrylate can be made to polymerize in conjunction with water, cyano is added dropwise in the dispersion of calcium alginate gel and organic solvent After acrylate, cyanoacrylate spontaneous can adhere on cyst wall surface, and polymerisation occurs, and obtain the first water blocking layer;And And used organic solvent and water are immiscible, then do not penetrate into capsule sandwich layer, in sandwich layer water or aqueous components cause Pollution or undesirable influence.This method is different from that directly capsule being impregnated in covering material, or brushes, spray coating material Material forms the conventional method of water blocking layer.Conventional method is compared it is found that this method can be evenly coated, the glue that blocks water of good sphericity Capsule, improves the load water stability and effect of capsule, and largely reduces the dosage of the first water blocking layer raw material, very Suitable for industrialized production.
Efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, which is characterized in that the method for the second water blocking layer of cladding is, by step (2) in a solvent, which can not dissolve the first water blocking layer to gained capsules disperse, immiscible with light-cured resin and will not occur Reaction, solvent are water, dimethyl carbonate, butyl acetate, chloroform, silicone oil, petroleum ether, toluene, n-hexane, atoleine one Kind is several, light-cured resin monomer and initiator is added dropwise to above-mentioned dispersion while stirring, then cure using ultraviolet lighting Coat the second water blocking layer.
The present invention does not do particular determination to the type of light-cured resin and initiator, including those skilled in the art can It chooses, the photo-curing monomer not reacted with solvent, and the light-cured resin list of waterproof effect can be played after curing Body and initiator.
It can also select commercially available light-cured resin monomer TTA21P and initiator UVI6976.
Solvent used by step (2) of the present invention is water, dimethyl carbonate, butyl acetate, chloroform, silicone oil, oil Ether, toluene, n-hexane, atoleine are one or more of, and above-mentioned solvent will not dissolve the first water blocking layer, and it is solid not interfere with light Change resin monomer polymerisation.This method is different from that directly capsule being added in light-cured resin to impregnate, or brushes, spraying Light-cured resin forms the conventional method of water blocking layer.Conventional method is compared it is found that the smooth circle of capsule surface prepared by this method Profit, is evenly coated, good sphericity, and the load water stability of capsule is high, and Storage period is long, and largely reduces second and block water The dosage of layer raw material is conducive to industrialized production popularization.
Efficient anti-seepage leakage prepared by the present invention carries capsule with diuresis promoting function and can apply to food, medicine and Cigarette processing field.
The capsule being prepared using the method for the present invention, manufacturing process is easy, and ratio of briquetting is high, and uniform particle sizes are simultaneously easy control System, block water impermeable excellent ability, there is longer Storage period, can be used for food, medicine and Cigarette processing field.
Description of the drawings
Fig. 1:Capsule structure schematic diagram
1:Sandwich layer;2:Cyst wall layer;3:First water blocking layer;4:Second water blocking layer
Fig. 2;Capsule microscope figure a, pure calcium alginate carry capsule with diuresis promoting function;B, the capsule prepared using the method for comparative example 3;C, The capsule prepared using embodiment 6
Specific embodiment
Embodiment 1
A kind of efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, follows the steps below making:Sandwich layer is prepared, sandwich layer is Calcium chloride water, a concentration of 10%;Prepare cyst wall layer, cyst wall layer raw material be sodium alginate soln, a concentration of 3%;Prepare the One water blocking layer, the first water blocking layer are cyanoacrylate.Operating procedure is that (1) prepares capsule by the anti-method of dripping, and sandwich layer is chlorination Calcium aqueous solution, cyst wall layer raw material are sodium alginate soln;(2) capsules disperse obtained by step (1) is in dimethyl carbonate, to above-mentioned Cyanoacrylate is added dropwise in dispersion, until capsule surface forms the first water blocking layer.In order to ensure alginic acid when preparing capsule The mobility of sodium, temperature are controlled at 60 DEG C.
Embodiment 2
A kind of efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, follows the steps below making:Prepare sandwich layer, sandwich layer For the mixed solution of water, essence and calcium chloride, essence a concentration of 20%, calcium chloride solution concentration 10%;Prepare cyst wall layer, capsule Parietal layer raw material be sodium alginate soln, a concentration of 3%;The first water blocking layer is prepared, the first water blocking layer is cyanoacrylate;It prepares Second water blocking layer, the second water blocking layer are the mixed solution of light-cured resin monomer and initiator.Operating procedure is that (1) is by anti- Drop method prepares capsule, and sandwich layer is the mixed solution of water, essence and calcium chloride, and cyst wall layer raw material is sodium alginate soln;(2) capsule Surface coats the first water blocking layer, and by capsules disperse obtained by step (1) in dimethyl carbonate, cyano is added dropwise to above-mentioned dispersion Acrylate, until forming the first water blocking layer;(3) the efficient anti-seepage leakage being prepared in step (2) carries capsule with diuresis promoting function surface and coats Light-cured resin monomer is added dropwise in toluene, to above-mentioned dispersion in second water blocking layer, i.e., the capsules disperse obtained (2) step With the mixed solution of initiator, it is stirred to react a period of time, until forming the second water blocking layer.In order to ensure seaweed when preparing capsule The mobility of sour sodium, temperature are controlled at 60 DEG C.
Embodiment 3
A kind of efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, follows the steps below making:Sandwich layer is prepared, sandwich layer is The mixed solution of water, essence and calcium chloride, essence a concentration of 20%, calcium chloride solution concentration 10%;Prepare cyst wall layer, cyst wall Layer raw material be sodium alginate soln, a concentration of 3%;The first water blocking layer is prepared, the first water blocking layer is cyanoacrylate;Prepare the Two water blocking layers, the second water blocking layer are the mixed solution of light-cured resin monomer and initiator.Operating procedure is that (1) is dripped by counter Method prepares capsule, and sandwich layer is the mixed solution of water, essence and calcium chloride, and cyst wall layer raw material is sodium alginate soln;(2) capsule table Bread covers the first water blocking layer, and by capsules disperse obtained by step (1) in butyl acetate, cyanoacrylate is added dropwise to above-mentioned dispersion Acid esters, until forming the first water blocking layer;(3) the efficient anti-seepage leakage being prepared in step (2) carries capsule with diuresis promoting function surface cladding second Light-cured resin monomer and initiation is added dropwise in water, to above-mentioned dispersion in water blocking layer, i.e., the capsules disperse obtained (2) step The mixed solution of agent is stirred to react a period of time, until forming the second water blocking layer.In order to ensure sodium alginate when preparing capsule Mobility, temperature are controlled at 60 DEG C.
Embodiment 4
A kind of efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, follows the steps below making:Prepare sandwich layer, sandwich layer For the mixed solution of water, essence and calcium chloride, essence a concentration of 15%, calcium chloride solution concentration 10%;Prepare cyst wall layer Solution, cyst wall layer raw material are sodium alginate soln, sodium alginate soln a concentration of 3%;Prepare the first water blocking layer, the first water blocking layer For cyanoacrylate;The second water blocking layer is prepared, the second water blocking layer is the mixed solution of light-cured resin monomer and initiator.Behaviour It is that (1) prepares capsule by the anti-method of dripping as step, sandwich layer is the mixed solution of water, essence and calcium chloride, and cyst wall layer raw material is sea Solution of sodium alginate;(2) capsule surface coats the first water blocking layer, by step (1) gained capsules disperse in petroleum ether, to above-mentioned point Cyanoacrylate is added dropwise in granular media system, until forming the first water blocking layer;(3) efficient anti-seepage being prepared in step (2), which leaks, carries Capsule with diuresis promoting function surface coats the second water blocking layer, i.e., the capsules disperse obtained (2) step is dripped in n-hexane to above-mentioned dispersion The mixed solution for adding light-cured resin monomer and initiator is stirred to react a period of time, until forming the second water blocking layer.Prepare glue When capsule, in order to ensure that the mobility of sodium alginate soln, temperature are controlled at 60 DEG C.
Embodiment 5
A kind of efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, follows the steps below making:Sandwich layer is prepared, sandwich layer is The mixed solution of water, essence and calcium chloride, essence a concentration of 15%, calcium chloride solution concentration 10%;Prepare cyst wall layer, cyst wall Layer raw material be sodium alginate soln, a concentration of 3%;The first water blocking layer is prepared, the first water blocking layer is cyanoacrylate;Prepare the Two water blocking layers, the second water blocking layer are the mixed solution of light-cured resin monomer and initiator.Operating procedure is that (1) is dripped by counter Method prepares capsule, and sandwich layer is the mixed solution of water, essence and calcium chloride, and cyst wall layer raw material is sodium alginate soln;(2) capsule table Bread covers the first water blocking layer, and by capsules disperse obtained by step (1) in dimethyl carbonate, cyano third is added dropwise to above-mentioned dispersion Olefin(e) acid ester type compound, until forming the first water blocking layer;(3) the efficient anti-seepage leakage being prepared in step (2) carries capsule with diuresis promoting function table Bread covers the second water blocking layer, i.e., photocuring tree is added dropwise in silicone oil, to above-mentioned dispersion in the capsules disperse obtained (2) step The mixed solution of alicyclic monomer and initiator is stirred to react a period of time, until forming the second water blocking layer.When preparing capsule, in order to Ensure that the mobility of sodium alginate soln, temperature are controlled at 60 DEG C.
Embodiment 6
A kind of efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, follows the steps below making:Sandwich layer is prepared, sandwich layer is The mixed solution of water, essence, calcium chloride and chitosan, essence a concentration of 10%, calcium chloride solution concentration 10%, chitosan is molten Liquid concentration 1%;Cyst wall layer is prepared, the raw material of cyst wall layer is sodium alginate soln, sodium alginate soln a concentration of 3%;Prepare the One water blocking layer, the first water blocking layer are cyanoacrylate;Prepare the second water blocking layer, the second water blocking layer be light-cured resin monomer with The mixed solution of initiator.Operating procedure is that (1) prepares capsule by the anti-method of dripping, and sandwich layer is that water, essence, calcium chloride and shell are poly- The mixed solution of sugar, cyst wall layer raw material are sodium alginate soln;(2) capsule surface coats the first water blocking layer, obtained by step (1) Cyanoacrylate compound is added dropwise in dimethyl carbonate, to above-mentioned dispersion in capsules disperse, until forming the first resistance Water layer;(3) the efficient anti-seepage leakage being prepared in step (2) carries capsule with diuresis promoting function surface and coats the second water blocking layer, i.e., obtains (2) step To capsules disperse in toluene, to above-mentioned dispersion be added dropwise light-cured resin monomer and initiator mixed solution, stirring Reaction a period of time, until forming the second water blocking layer.When preparing capsule, in order to ensure the mobility of sodium alginate soln, temperature Control is at 60 DEG C.
Embodiment 7
A kind of efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, follows the steps below making:Sandwich layer is prepared, sandwich layer is The mixed solution of water, essence, calcium chloride and chitosan, essence a concentration of 10%, calcium chloride solution concentration 10%, chitosan is molten Liquid concentration 1%;Cyst wall layer is prepared, the raw material of cyst wall layer is sodium alginate soln, sodium alginate soln a concentration of 3%;Prepare the One water blocking layer, the first water blocking layer are Instant cement 502;The second water blocking layer is prepared, the second water blocking layer is light-cured resin monomer The mass ratio of the mixed solution of TTA21P and initiator UVI6976, TTA21P and UVI6976 are 100:4.Operating procedure is (1) Capsule is prepared by the anti-method of dripping, sandwich layer is the mixed solution of water, essence, calcium chloride and chitosan, and cyst wall layer raw material is alginic acid Sodium solution;(2) capsule surface coats the first water blocking layer, by step (1) gained capsules disperse in dimethyl carbonate, to above-mentioned point Instant cement 502 is added dropwise in granular media system, until forming the first water blocking layer;(3) the efficient anti-seepage leakage being prepared in step (2) carries glue Capsule surface coats the second water blocking layer, i.e., the capsules disperse obtained (2) step is added dropwise in atoleine to above-mentioned dispersion The mixed solution of TTA21P and UVI6976 is stirred to react a period of time, until forming the second water blocking layer.When preparing capsule, in order to Ensure that the mobility of sodium alginate soln, temperature are controlled at 60 DEG C.
Embodiment 8
A kind of efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, follows the steps below making:Sandwich layer is prepared, sandwich layer is The mixed solution of water, essence, calcium chloride and chitosan, essence a concentration of 10%, calcium chloride solution concentration 10%, chitosan is molten Liquid concentration 1%;Cyst wall layer is prepared, the raw material of cyst wall layer is sodium alginate soln, sodium alginate soln a concentration of 3%;Prepare the One water blocking layer, the first water blocking layer are the mixture of Instant cement 502 and Instant cement 508, and 502 and 508 mass ratio is 1:1;It prepares Second water blocking layer, the second water blocking layer be light-cured resin monomer TTA21P and initiator UVI6976 mixed solution, TTA21P and The mass ratio of UVI6976 is 100:0.4.Operating procedure is that (1) prepares capsule by the anti-method of dripping, and sandwich layer is water, essence, chlorination The mixed solution of calcium and chitosan, cyst wall layer raw material are sodium alginate soln;(2) capsule surface coats the first water blocking layer, will walk Suddenly the mixing of Instant cement 502 and Instant cement 508 is added dropwise to above-mentioned dispersion in dimethyl carbonate for capsules disperse obtained by (1) Object, until forming the first water blocking layer;(3) the efficient anti-seepage leakage being prepared in step (2) carries the second resistance of capsule with diuresis promoting function surface cladding TTA21P and UVI6976 is added dropwise in atoleine, to above-mentioned dispersion in water layer, i.e., the capsules disperse obtained (2) step Mixed solution, be stirred to react a period of time, until formed the second water blocking layer.When preparing capsule, in order to ensure that sodium alginate is molten The mobility of liquid, temperature are controlled at 60 DEG C.
Comparative example 1
A kind of preparation method of capsule, follows the steps below making:Sandwich layer is prepared, sandwich layer is water;Cyst wall layer is prepared, Cyst wall layer raw material be sodium alginate soln, a concentration of 3%;Coagulating bath is calcium chloride solution, a concentration of 10%.Operating procedure is, Capsule is prepared by the just method of dripping, sandwich layer is water, and cyst wall layer raw material is sodium alginate soln.When preparing capsule, in order to ensure seaweed The mobility of sour sodium, control are 60 DEG C in temperature.
Comparative example 2
A kind of efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, follows the steps below making:Prepare sandwich layer, sandwich layer For water;Preparing cyst wall layer, cyst wall layer raw material is sodium alginate soln, a concentration of 3%;Coagulating bath is calcium chloride solution, concentration It is 10%;Water blocking layer is prepared, water blocking layer is beeswax, paraffin and Brazil wax, wherein beeswax 50%, paraffin 40%, cohune Palmitic acid wax 10%.Operating procedure is that (1) prepares capsule by the just method of dripping, and sandwich layer is water, and cyst wall layer raw material is sodium alginate soln; (2) capsule surface coats water blocking layer, and water blocking layer is beeswax 50%, paraffin 40%, Brazil wax 10%, and capsule is being mixed above It closes in wax and handles 1min, then carry out low temperature solidification;When preparing capsule, in order to ensure that the mobility of sodium alginate, temperature control exist 60 DEG C, in order to ensure that the mobility of blended wax, temperature are controlled at 80 DEG C.
Comparative example 3
A kind of efficient anti-seepage leakage carries the preparation method of capsule with diuresis promoting function, follows the steps below making:Prepare sandwich layer, sandwich layer For water and essence, essence a concentration of 20%;Prepare cyst wall layer, cyst wall layer raw material be sodium alginate soln, a concentration of 3%;Solidification It is calcium chloride solution to bathe, a concentration of 10%;The first water blocking layer is prepared, the first water blocking layer is cyanoacrylate, the second water blocking layer For light-cured resin.Operating procedure is that (1) prepares capsule by the just method of dripping, and sandwich layer is essence aqueous solution, and cyst wall layer raw material is sea Solution of sodium alginate;(2) capsule surface coats the first water blocking layer, and capsule obtained by step (1) is added in cyanoacrylate, reaction Until forming the first water blocking layer;(3) capsule surface being prepared in step (2) coats the second water blocking layer, i.e., obtains (2) step To capsule be added in the mixed solution of light-cured resin monomer and initiator, reaction is until form the second water blocking layer.Prepare glue In order to ensure the mobility of sodium alginate when capsule, temperature control is at 60 DEG C.
Capsule in above-described embodiment and comparative example is tested, the performance of capsule under different factors is compared.
Capsule diameter
10 capsules are taken at random, after blotting surface moisture with filter paper, every capsule is measured by digimatic calipers Maximum particle diameter DmaxWith minimum grain size Dmin, record and calculate average grain diameter D;
Sphericity SF
By measuring the diameter of capsule, sphericity is calculated.
Its formula is:SF=(Dmax–Dmin)/(Dmax+Dmin);SF value variation ranges are 0-1, and SF values are smaller, capsule shape Closer to spherical.SF values are bigger, and capsule shape deviates spherical.Usually with SF<0.07 standard spherical in shape as capsule is judged.
Intensity
It is tested using DWY-iii dripping pill quality comprehensive testers;Since the capsule of the present invention can be used for cigarette field, because This, it is desirable that capsule is easy to pinch brokenly, and intensity is between 10-16N.
Silica gel colour developing test
The principle of water discoloration, the anti-permeability of test capsule are met using silica gel, specific test method is:Randomly select 50 Capsule, is placed in sample bottle, and 50 discoloration silica gel are added, and the sample bottle equipped with sample and discoloration silica gel is placed in dry by sealing In dry device, under the conditions of 25 DEG C, the color change of silica gel in sample bottle is observed at regular intervals.Coloring Time is measured to ooze to characterize Water effect, testing time are 30 days, and observation whether there is discoloration in 30 days.
Permeability rate
20 capsules are randomly selected, are positioned in open environment, the weight-loss ratio of its 7 days and 30 days, as permeability rate are tested.
Table 1:Each results of property of capsule
Embodiment 13:The capsule that embodiment 6 is prepared, is added in cigaratte filter, and the perfume (or spice) containing quick-fried pearl is prepared Cigarette filter tip.
Embodiment 14:The capsule that embodiment 1 is prepared, as drug capsule.
Embodiment 15:The capsule that embodiment 1 is prepared, as food additives, as food capsule.

Claims (9)

1. a kind of efficient anti-seepage leakage carries capsule with diuresis promoting function, it is characterised in that:Capsule is at least three-decker, is followed successively by core from inside to outside Layer, cyst wall layer, the first water blocking layer, first water blocking layer are coated on outside cyst wall layer, are one or more cyanoacrylates The polymerizate of compound, the efficient anti-seepage leakage carry 7 days permeability rates of capsule with diuresis promoting function and are less than 4%, sphericity SF<0.07.
2. a kind of efficient anti-seepage as described in claim 1 leakage carries capsule with diuresis promoting function, it is characterised in that capsule further includes the 4th layer, and the 4th Layer is the second water blocking layer, and the second water blocking layer is coated on outside the first water blocking layer, and the second water blocking layer is light-cured resin.
3. a kind of as the leakage of claim 1-2 any one of them efficient anti-seepages carries capsule with diuresis promoting function, which is characterized in that sandwich layer is water or contains Water component.
4. a kind of as the leakage of claim 1-2 any one of them efficient anti-seepages carries capsule with diuresis promoting function, which is characterized in that the cyst wall layer is It is one or more in alginate, cellulose derivative, gelatin, chitosan, polyethylene glycol, polyvinyl alcohol.
5. a kind of efficient anti-seepage leakage according to any one of claims 1-4 carries the preparation method of capsule with diuresis promoting function, it is characterised in that packet Include following steps:(1) capsule is prepared by dropping preparation method, sandwich layer is water or aqueous components, and cyst wall layer is alginate, cellulose spreads out It is one or more in biology, gelatin, chitosan, polyethylene glycol, polyvinyl alcohol;(2) capsule surface coats the first water blocking layer; (3) the efficient anti-seepage leakage being prepared in step (2) carries capsule with diuresis promoting function surface and coats the second water blocking layer.
6. a kind of efficient anti-seepage leakage as claimed in claim 5 carries the preparation method of capsule with diuresis promoting function, which is characterized in that the dropping preparation method Method is dripped to be counter, temperature when preparing capsule is 50-80 DEG C.
7. a kind of efficient anti-seepage leakage as claimed in claim 5 carries the preparation method of capsule with diuresis promoting function, which is characterized in that the first resistance of cladding The method of water layer is, by capsules disperse obtained by step (1), in a solvent, the solvent and water are immiscible, and not with cyanoacrylate Acid esters compound reacts, solvent be dimethyl carbonate, butyl acetate, chloroform, silicone oil, petroleum ether, toluene, just oneself Cyanoacrylate compound is added dropwise to dispersion in one or more of alkane, atoleine, blocks water until forming first Layer.
8. a kind of efficient anti-seepage leakage as claimed in claim 5 carries the preparation method of capsule with diuresis promoting function, which is characterized in that the second resistance of cladding The method of water layer is that in a solvent, which can not dissolve the first water blocking layer, with photocuring by capsules disperse obtained by step (2) Resin is immiscible and will not react, and solvent is water, dimethyl carbonate, butyl acetate, chloroform, silicone oil, petroleum ether, first One or more of benzene, n-hexane, atoleine are added dropwise light-cured resin monomer to above-mentioned dispersion while stirring and draw Agent is sent out, then using ultraviolet lighting solidification the second water blocking layer of cladding.
9. a kind of application carrying capsule with diuresis promoting function such as the leakage of claim 1-8 any one of them efficient anti-seepages, it is characterised in that:By capsule For food, medicine, Field of Tobacco.
CN201810684856.3A 2018-06-28 2018-06-28 A kind of leakage of efficient anti-seepage carries capsule with diuresis promoting function and preparation method thereof Withdrawn CN108783554A (en)

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CN109567261A (en) * 2018-11-27 2019-04-05 江苏万腾新材料科技有限公司 Using water-soluble material as three layers of cigarette capsule of core material and preparation method thereof
CN110419774A (en) * 2019-07-10 2019-11-08 云南巴菰生物科技有限公司 A kind of quick-fried pearl of water and preparation method thereof with double rubber layers
CN110961056A (en) * 2019-11-18 2020-04-07 湖北中烟工业有限责任公司 Water-carrying capsule capable of giving out brittle sound and containing hydrophilic silicon dioxide and preparation method thereof

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CN110841566B (en) * 2019-11-18 2021-11-05 湖北中烟工业有限责任公司 High-efficiency anti-seepage water-carrying capsule capable of giving out brittle sound
CN111205838A (en) * 2020-02-26 2020-05-29 西南石油大学 Composite microcapsule for fractured rock mass solidification seepage prevention and preparation method thereof
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CN109567261A (en) * 2018-11-27 2019-04-05 江苏万腾新材料科技有限公司 Using water-soluble material as three layers of cigarette capsule of core material and preparation method thereof
CN110419774A (en) * 2019-07-10 2019-11-08 云南巴菰生物科技有限公司 A kind of quick-fried pearl of water and preparation method thereof with double rubber layers
CN110961056A (en) * 2019-11-18 2020-04-07 湖北中烟工业有限责任公司 Water-carrying capsule capable of giving out brittle sound and containing hydrophilic silicon dioxide and preparation method thereof

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