CN108041674A - A kind of impermeable capsule and preparation method thereof that efficiently blocks water - Google Patents

Abstract

The present invention relates to a kind of impermeable capsules and preparation method thereof that efficiently blocks water, capsule is at least three-decker, sandwich layer, cyst wall layer, water blocking layer are followed successively by from inside to outside, water blocking layer coats cyst wall layer, its material includes polyurethane, epoxy resin, acrylate, the one or more of isocyanates, water blocking layer can be chemically reacted with cyst wall layer, and the permeability rate of 7 days of the impermeable capsule that efficiently blocks water is less than 4%, sphericity SF<0.07, capsule prepared by this method, ratio of briquetting is high, and uniform particle diameter, block water impermeable excellent ability, and Storage period is long, and manufacturing process is easy, can be directly used for food, medicine and cigarette products processing.

Description

A high-efficiency water-blocking and anti-penetration capsule and its preparation method

technical field

The invention belongs to the field of capsule preparation, and in particular relates to a high-efficiency water-blocking and anti-penetration capsule.

Background technique

Encapsulation technology is used to wrap and seal water or water-soluble active ingredients to form capsules, so as to keep the water in the capsules free of leakage during long-term storage during transportation and shelf life. It has always been a research hotspot and difficulty in the fields of food, medicine, and tobacco.

The choice of capsule wall material determines the mechanical properties and permeability of the capsule. Calcium alginate is the most commonly used wall material in food and medicinal capsules. Calcium alginate capsules prepared by the dropping method using calcium ion solution as a coagulation bath have been put into industrial production and commercialized.

In the prior art, there are many reports on calcium alginate capsules coated with oil or oil-soluble active ingredients, but few reports on calcium alginate capsules containing water.

The existing invention patent, the publication number is CN102108136B, discloses a drop pill wrapping material for cigarette additives, the drop pill wrapped with it and the application of the drop pill, specifically discloses that the drop pill is used in the field of cigarettes, and is made by the positive drop method The capsule includes two layers, a core layer and a wrapping layer. The wrapping material is composed of sodium alginate: glycerin: water in a ratio of (1-8): (0.5-5): (85-100), and then mixed with solidified The calcium ions in the bath solidify to produce capsules. However, in the process of repeated experiments, we found that the wall of the capsule prepared by this method is very thin, does not have the mechanical strength required for subsequent industrial processing, and is relatively poor in practicability.

The existing invention patent, the publication number is CN103815541A, discloses a three-layer water-for-cigarette capsule, wherein the inner layer is water, gelatin, preservative and essence, the middle layer is sodium alginate, water, preservative, and the outer layer is beeswax, Made of paraffin wax and Brazilian wax. This invention wraps the mixed wax on the outer layer of the original calcium alginate capsule, which has a certain effect on preventing the water in the capsule from overflowing, but the interfacial binding force between the hydrophilic calcium alginate capsule wall layer and the lipophilic mixed wax layer is poor, The package is uneven and easily damaged, and the melting temperature of the mixed wax is around 50°C, which is easily affected by the external temperature and the state is unstable. These all cause this invention capsule to be unable to store for a long time, easy to leak.

The existing patent publication number is CN103815542A. On the basis of the above-mentioned invention patent, a four-layer water-for-smoking capsule is disclosed. A protective film to reduce wax breakage. However, the problem of poor interfacial bonding between sodium alginate and wax layer is still the main factor affecting the permeability of the capsule, resulting in the uneven wrapping of the third and fourth layers of the four-layer water capsule, which is easy to break and water seepage.

From the perspective of the prior art, there is already a technical solution for the preparation of water-blocking and anti-penetration capsules. A water-blocking layer is provided on the outer layer of the capsule to prevent the water or aqueous solution from the inner layer of the capsule from seeping out and prolong the service life of the capsule. In the prior art, only waxy materials are mostly used as the waterproof layer, and its effect is not ideal.

Contents of the invention

In view of the deficiencies in the prior art, the purpose of the present invention is to provide a high-efficiency water-blocking and anti-penetration capsule and a preparation method thereof. The invention solves the technical problems in the prior art that the water or aqueous solution of the capsule core layer is easy to permeate and the water blocking effect is not ideal.

In order to achieve the above object, the present invention provides a high-efficiency water-blocking and anti-penetration capsule, which is characterized in that: the capsule has a structure of at least three layers. The water-blocking layer is coated on the capsule wall layer, and its material is one or more of polyurethane, epoxy resin, acrylate, and isocyanate. The water permeability of the high-efficiency water-blocking and anti-penetration capsule for 7 days is less than 4%, and the sphericity SF< 0.07.

The first water blocking layer preferably includes one or more of epoxy resin, polyurethane, isocyanate and acrylate.

Further, the acrylate is water-curable acrylate, and the polyurethane is water-curable polyurethane.

Further isocyanates are diisocyanates, including toluene diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI), hexamethylene diisocyanate One or more of (HMDI), lysine diisocyanate (LDI).

The first water-blocking layer can chemically react with the wall layer, and further, the first water-blocking layer can chemically react with the moisture in the wall layer and firmly adhere to the wall layer, especially the wall layer. The rough parts in the layer, such as holes and depressions, the first water-blocking layer can go deep into these rough parts, making the wall layer more compact, and can effectively prevent the penetration of water in the wall layer; in addition, the first water-blocking layer itself is also It can form a dense film layer to prevent the penetration of water and achieve the effect of water blocking. In the present invention, a waxy layer can also be added on the outer layer of the first water-blocking layer as the fourth layer, that is, the second water-blocking layer. Although the waxy layer does not chemically react with the third layer, the waxy layer and the same The interfacial binding force between the hydrophobic third waterproof layer is better, which can further improve the water blocking effect. For the capsule prepared by the present invention, due to the obvious improvement of the capsule wall layer and the joint action of the first water blocking layer and the second water blocking layer, the structure and performance of the capsule are significantly changed, and the water permeability is greatly reduced. Enhanced water blocking effect.

The water permeability is tested by weighing method. Specifically, 50 capsules are randomly selected, weighed at intervals, and the weight loss rate is calculated, and the average value is taken. The result reflects the anti-seepage effect of the capsule, that is, the water permeability. The 7-day water permeability of the capsules prepared by the present invention is less than 4%, preferably less than 3%, more preferably less than 2%; the 30-day water permeability is less than 8%, preferably less than 5%, more preferably less than 3%.

The second water-blocking layer of the high-efficiency water-blocking and anti-penetration capsule is coated on the first water-blocking layer, and the second water-blocking layer is one or more of paraffin wax, beeswax or carnauba wax.

The waxy layer of the second water blocking layer can further reduce the water permeability of the capsule.

The first water-blocking layer or (and) the second water-blocking layer of the high-efficiency water-blocking and anti-penetration capsule also includes inorganic salts, and the inorganic salts are one or more of carbonates, sulfates, and silicates, and further , the first water blocking layer also includes inorganic salt, and the inorganic salt is gypsum.

Inorganic salts are added to the first water-blocking layer or (and) the second water-blocking layer. This type of inorganic salt can absorb the moisture in the wall layer and fill the rough surface of the wall layer. Further, the inorganic salt can React with the water in the capsule wall layer, improve the interface bonding force between the water blocking layer and the capsule wall layer or the water blocking layer, and strengthen the overall structure and water blocking performance of the capsule shell.

The core layer of the high-efficiency water-blocking and anti-penetration capsule is water or a water-containing component.

Further preferably, the aqueous component contains a solute of metal ions.

According to the actual application of the capsule, different core layer materials can be added, and the core layer can be water or a water-containing component. For a class of solutes containing metal ions, this type of solute can ion-exchange with the raw material of the wall layer, especially sodium alginate, to obtain a wall layer with a cross-linked structure, and effectively wrap the core layer of water or water-containing components A spherical capsule structure is formed.

The high-efficiency water-blocking and anti-penetration capsule is characterized in that the capsule wall layer is one or more of alginate, cellulose derivatives, gelatin, chitosan, polyethylene glycol, and polyvinyl alcohol.

In order to prepare the capsule of the present invention, the preparation method of the present invention comprises the following steps: (1) prepare the capsule by dropping method, the core layer is water or water-containing component, and the capsule wall layer is alginate, cellulose derivative, gelatin, Chitosan, polyethylene glycol, polyvinyl alcohol; (2) the surface of the capsule is coated with the first water-blocking layer; (3) the surface of the high-efficiency water-blocking and anti-penetration capsule prepared in step (2) is coated with the second water-blocking layer .

The method for preparing high-efficiency water-blocking and anti-penetration capsules is characterized in that the dripping method is a back-dropping method, and the temperature for preparing the capsules is 50-80°C.

Capsules can be prepared by the forward drop method and the reverse drop method. The forward drop method is to drop the capsule wall material and the core layer material into the coagulation solution through a coaxial double-needle dropping device. The capsule prepared by the forward drop method has a capsule wall layer The crosslinking reaction is the diffusion process from the outer wall to the core layer. The back-drop method is to drop the solution containing the coagulation component into the raw material of the wall layer of the capsule, and the cross-linking reaction of the wall of the capsule prepared by the back-drop method is a process of diffusion from the core layer to the wall layer. The dropping order of the forward drop method and the reverse drop method are different, so that the curing degree of the capsule wall layer is different. The size of the capsule prepared by the reverse drop method is easier to control, and the thickness of the capsule wall is large, which can prevent the seepage of water and also It can meet the requirements of capsule crushing strength in subsequent processing. The diameter of capsules prepared by positive drop method is 3+2mm.

The high-efficiency water-blocking and anti-penetration capsule prepared by the invention can be applied to the fields of food, medicine and cigarette processing.

The capsule prepared by the method of the invention has simple manufacturing process, high forming rate, uniform particle size and easy control, excellent water blocking and anti-penetration ability, long storage period, and can be directly used in the fields of food, medicine and cigarette processing.

Description of drawings

Figure 1: Schematic diagram of capsule structure

1: core layer; 2: capsule wall layer; 3: first water blocking layer; 4: second water blocking layer

Figure 2; Capsule microscope image

specific embodiment

Example 1

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: preparing a core layer, the core layer is deionized water; preparing a capsule wall layer, and the raw material of the capsule wall layer is sodium alginate solution with a concentration of 3%; coagulation bath Calcium chloride solution with a concentration of 10%; prepare the first water blocking layer, the first water blocking layer is toluene diisocyanate, and the second water blocking layer is a mixture of paraffin wax, beeswax and carnauba wax. The operation steps are as follows: (1) Capsules are prepared by the positive drop method, the core layer is deionized water, and the raw material of the capsule wall layer is sodium alginate solution; (2) the surface of the capsules is coated with the first water blocking layer, and the prepared capsules are washed with water Put it into the first water-blocking layer; (3) The surface of the high-efficiency water-blocking and anti-penetration capsule prepared in step (2) is coated with the second water-blocking layer, that is, the capsule obtained in step (2) is put into paraffin wax, beeswax in a mixture with carnauba wax. In order to ensure the fluidity of the sodium alginate when preparing the capsules, the temperature was controlled at 60°C, and in order to ensure the fluidity of the waxy mixture, the temperature was controlled at 80°C.

Example 2

A method for preparing a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: prepare a core layer, the core layer is water and essence, and the essence concentration is 20%; prepare a capsule wall layer, the raw material of the capsule wall layer is sodium alginate solution, The concentration is 3%; the coagulation bath is calcium chloride solution, the concentration is 10%; the first water blocking layer is prepared, the first water blocking layer is toluene diisocyanate, and the second water blocking layer is a mixture of paraffin wax, beeswax and carnauba wax . The operation steps are as follows: (1) Capsules are prepared by the positive drop method, the core layer is an aqueous essence solution, and the raw material of the capsule wall layer is sodium alginate solution; (2) The surface of the capsule is coated with the first water-blocking layer, and the prepared capsule is washed and placed (3) The surface of the high-efficiency water-blocking and anti-penetration capsule prepared in step (2) is coated with the second water-blocking layer, that is, the capsule obtained in step (2) is put into the mixed wax. In order to ensure the fluidity of the sodium alginate when preparing the capsules, the temperature was controlled at 60°C, and in order to ensure the fluidity of the mixed wax, the temperature was controlled at 80°C.

Example 3

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: preparing a core layer, the core layer is water and essence, and the concentration of the essence is 20%; preparing a capsule wall layer, the raw material of the capsule wall layer is sodium alginate solution, the concentration 3%; the coagulation bath is calcium chloride solution, the concentration is 10%; the first water-blocking layer is prepared, and the first water-blocking layer is one-component water-cured polyurethane; the second water-blocking layer is paraffin, beeswax and carnauba wax mixture. The operation steps are as follows: (1) Capsules are prepared by the positive drop method, the core layer is an aqueous essence solution, and the raw material of the capsule wall layer is sodium alginate solution; (2) The surface of the capsule is coated with the first water-blocking layer, and the prepared capsule is washed and placed (3) The surface of the high-efficiency water-blocking and anti-penetration capsule prepared in step (2) is coated with the second water-blocking layer, that is, the capsule obtained in step (2) is put into the mixed wax. In order to ensure the fluidity of the sodium alginate when preparing the capsules, the temperature was controlled at 60°C, and in order to ensure the fluidity of the mixed wax, the temperature was controlled at 80°C.

Example 4

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: preparing a core layer, the core layer is water and essence, and the concentration of the essence is 20%; preparing a capsule wall layer, the raw material of the capsule wall layer is sodium alginate solution, the concentration 3%; the coagulation bath is calcium chloride solution, the concentration is 10%; the first water-blocking layer is prepared, and the first water-blocking layer is a mixture of one-component water-curable polyurethane and calcium silicate; the second water-blocking layer is paraffin , a blend of beeswax and carnauba wax. The operation steps are as follows: (1) Capsules are prepared by the positive drop method, the core layer is an aqueous essence solution, and the raw material of the capsule wall layer is a sodium alginate solution; (2) the surface of the capsules is coated with a first water-blocking layer, and the prepared capsules are washed with water. Putting it into the first water-blocking layer; (3) coating the surface of the high-efficiency water-blocking and anti-penetration capsule prepared in step (2) with the second water-blocking layer, that is, putting the capsule obtained in step (2) into the paraffin solution. In order to ensure the fluidity of the sodium alginate solution when preparing the capsules, the temperature was controlled at 60° C., and in order to ensure the fluidity of the mixed wax, the temperature was controlled at 80° C.

Example 5

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: a core layer is prepared, the core layer is water and essence, and the essence concentration is 15%; a capsule wall layer solution is prepared, and the raw material of the capsule wall layer is sodium alginate solution, the concentration of sodium alginate solution is 3%; the coagulation bath is calcium chloride solution, the concentration is 10%; the first water blocking layer is prepared, and the first water blocking layer is a mixture of one-component water-curable polyurethane and calcium silicate, The second water blocking layer is a mixture of paraffin wax, beeswax, carnauba wax and calcium silicate. The operation steps are as follows: (1) Capsules are prepared by the positive drop method, the core layer is an aqueous essence solution, and the raw material of the capsule wall layer is a sodium alginate solution; (2) the surface of the capsules is coated with a first water-blocking layer, and the prepared capsules are washed with water. Put it into the first water-blocking layer; (3) The surface of the high-efficiency water-blocking and anti-penetration capsule prepared in step (2) is coated with the second water-blocking layer, that is, the capsule obtained in step (2) is put into wax and silicic acid calcium mixture. When preparing the capsules, in order to ensure the fluidity of the sodium alginate solution, the temperature was controlled at 60° C., and in order to ensure the fluidity of the mixture of wax and calcium silicate, the temperature was controlled at 80° C.

Example 6

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: preparing a core layer, the core layer is water and essence, and the concentration of the essence is 15%; preparing a capsule wall layer, the raw material of the capsule wall layer is sodium alginate solution, the concentration 3%; the coagulation bath is calcium chloride solution, the concentration is 10%; the first water-blocking layer is prepared, the first water-blocking layer is modified water-cured acrylate, and the second water-blocking layer is paraffin wax, beeswax and carnauba wax mixture. The operation steps are as follows: (1) Capsules are prepared by the positive drop method, the core layer is an aqueous essence solution, and the raw material of the capsule wall layer is a sodium alginate solution; (2) the surface of the capsules is coated with a first water-blocking layer, and the prepared capsules are washed with water. Putting it into the first water-blocking layer; (3) coating the surface of the high-efficiency water-blocking and anti-penetration capsule prepared in step (2) with the second water-blocking layer, that is, putting the capsule obtained in step (2) into the mixed wax. When preparing the capsules, in order to ensure the fluidity of the sodium alginate solution, the temperature was controlled at 60°C, and in order to ensure the fluidity of the mixed wax, the temperature was controlled at 80°C.

Example 7

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: preparing a core layer, the core layer is water and essence, and the essence concentration is 10%; preparing a capsule wall layer, and the raw material of the capsule wall layer is sodium alginate/shell Polysaccharide mixed solution, the concentration of sodium alginate solution is 3%, the concentration of chitosan solution is 1%; the coagulation bath is calcium chloride, the concentration is 10%; the first water blocking layer is prepared, and the first water blocking layer is modified water Cured acrylate, second water barrier layer is a mixture of paraffin, beeswax and carnauba wax. The operation steps are as follows: (1) Capsules are prepared by the positive drop method, the core layer is an aqueous essence solution, and the raw material of the capsule wall layer is a mixed solution of sodium alginate/chitosan; (2) the surface of the capsule is coated with the first water-blocking layer, and the prepared The obtained capsules are washed and put into the first water-blocking layer; (3) the surface of the high-efficiency water-blocking and anti-penetration capsules prepared in step (2) is coated with the second water-blocking layer, that is, the capsules obtained in step (2) are put into Mix in wax. When preparing the capsules, in order to ensure the fluidity of the sodium alginate/chitosan mixed solution, the temperature was controlled at 60°C, and in order to ensure the fluidity of the mixed wax, the temperature was controlled at 80°C.

Example 8

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: preparing a core layer, the core layer is calcium chloride solution, and the concentration is 10%; preparing a capsule wall layer, and the raw material of the capsule wall layer is sodium alginate solution, the concentration is 10%. 3%; prepare the first water-blocking layer, the first water-blocking layer is one-component water-cured polyurethane, and the second water-blocking layer is a mixture of paraffin wax, beeswax and carnauba wax. The operation steps are as follows: (1) prepare capsules by back-dropping method, the core layer is calcium chloride solution, and the raw material of capsule wall layer is sodium alginate solution; (2) the surface of the capsules is coated with the first water-blocking layer, and the prepared capsules are washed with water Then put it into the first water-blocking layer; (3) The surface of the high-efficiency water-blocking and anti-penetration capsule prepared in step (2) is coated with the second water-blocking layer, that is, the capsule obtained in step (2) is put into the mixed wax. When preparing the capsules, in order to ensure the fluidity of the sodium alginate solution, the temperature was controlled at 60°C, and in order to ensure the fluidity of the mixed wax, the temperature was controlled at 80°C.

Example 9

A method for preparing a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: preparing a core layer, the core layer is an aqueous solution, and the solution contains 20% essence and 0.5% calcium chloride; preparing a capsule wall layer, and the raw material of the capsule wall layer is alginic acid Sodium solution, the concentration of sodium alginate solution is 3%; the first water blocking layer is prepared, the first water blocking layer is water-cured modified acrylate, and the second water blocking layer is a mixture of paraffin wax, beeswax and carnauba wax. The operation steps are as follows: (1) Capsules are prepared by the reverse drop method, the core layer is a mixed solution of calcium chloride, essence and water, and the raw material of the capsule wall layer is sodium alginate solution; (2) The surface of the capsule is coated with the first water-blocking layer , wash the prepared capsules and put them into the first water-blocking layer; (3) The surface of the high-efficiency water-blocking and anti-penetration capsules prepared in step (2) is coated with the second water-blocking layer, that is, the capsules obtained in step (2) Put in the mixed wax. When preparing the capsules, in order to ensure the fluidity of the sodium alginate solution, the temperature was controlled at 60°C, and in order to ensure the fluidity of the mixed wax, the temperature was controlled at 80°C.

Example 10

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: preparing a core layer, the core layer is an aqueous solution, and the solute contains 20% essence and 0.1% calcium sulfate; preparing a capsule wall layer, and the raw material of the capsule wall layer is sodium alginate Solution, the concentration is 3%; prepare the first water blocking layer, the first water blocking layer is a mixture of water-curable modified acrylate and calcium sulfate, and the second water blocking layer is a mixture of paraffin wax, beeswax, carnauba wax and calcium carbonate . The operation steps are as follows: (1) prepare capsules by back-dropping method, the core layer is an aqueous solution, and the raw material of the capsule wall layer is sodium alginate solution; (2) the surface of the capsules is coated with the first water-blocking layer, and the prepared capsules are washed with water and put into In the first water-blocking layer; (3) the surface of the high-efficiency water-blocking and anti-penetration capsule prepared in step (2) is coated with the second water-blocking layer, that is, the capsule obtained in step (2) is put into a mixture of wax and calcium carbonate middle. When preparing the capsules, in order to ensure the fluidity of the sodium alginate solution, the temperature was controlled at 60°C, and in order to ensure the fluidity of the wax and calcium carbonate mixture, the temperature was controlled at 80°C.

Example 11

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: preparing a core layer, the core layer is an aqueous solution, and the solute contains 15% mint and 1% calcium sulfate; preparing a capsule wall layer, and the raw material of the capsule wall layer is sodium alginate Mixed solution with gelatin, the concentration of sodium alginate solution is 3%, and the concentration of gelatin solution is 1%; the first water-blocking layer is water-cured modified acrylate; the second water-blocking layer is a mixture of paraffin wax, beeswax and carnauba wax . The operation steps are as follows: (1) Capsules are prepared by the reverse drop method, the core layer is an aqueous solution, and the raw materials of the capsule wall layer are sodium alginate and gelatin; (2) the surface of the capsules is coated with the first water-blocking layer, and the prepared capsules are washed and placed into the water-cured modified acrylate; (3) the surface of the high-efficiency water-blocking and anti-penetration capsule prepared in step (2) is coated with a second water-blocking layer, that is, the capsule obtained in step (2) is put into the mixed wax. When preparing the capsules, in order to ensure the fluidity of the sodium alginate, the temperature was controlled at 60°C, and in order to ensure the fluidity of the mixed wax, the temperature was controlled at 80°C.

Example 12

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: prepare a core layer, the core layer is an aqueous solution, and the solute includes 1% naringin, 1% calcium sulfate and 1% carboxymethyl cellulose; prepare the capsule The wall layer solution, the material of the wall layer is a mixed solution of sodium alginate and chitosan, the concentration of the sodium alginate solution is 3%, and the concentration of the chitosan solution is 1%; prepare the first water blocking layer, the first water blocking layer It is a mixture of water-curable modified acrylate and calcium sulfate hydrate; the second water-blocking layer is a mixture of paraffin wax, beeswax and carnauba wax. The operation steps are as follows: (1) prepare the capsule by the back-drop method, the core layer is an aqueous solution, and the raw material of the capsule wall layer is a mixed solution of sodium alginate and chitosan; (2) the surface of the capsule is coated with the first water-blocking layer, and the capsule is Add it to the mixed solution of water-curable modified acrylate and calcium sulfate, stir for 10 minutes, filter, cure in an oven at 50°C for 1 hour, take it out for use; (3) Coat the high-efficiency water-blocking and anti-penetration capsule prepared in step (2) The second water blocking layer is to put the capsules obtained in step (2) into the mixed wax. When preparing capsules, in order to ensure the fluidity of the sodium alginate and chitosan mixed solution, the temperature was controlled at 60°C, and in order to ensure the fluidity of the mixed wax, the temperature was controlled at 80°C.

Comparative example 1

A preparation method of a capsule, which is produced according to the following steps: preparing a core layer, the core layer is water; preparing a capsule wall layer, the raw material of the capsule wall layer is a sodium alginate solution with a concentration of 3%; a coagulation bath is a calcium chloride solution, The concentration is 10%. The operation steps are as follows: the capsule is prepared by the positive drop method, the core layer is water, and the raw material of the capsule wall layer is sodium alginate solution. When preparing the capsules, in order to ensure the fluidity of the sodium alginate, the temperature is controlled at 60°C.

Comparative example 2

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: a core layer is prepared, and the core layer is water; a capsule wall layer is prepared, and the raw material of the capsule wall layer is sodium alginate solution with a concentration of 3%; a coagulation bath Calcium chloride solution with a concentration of 10%; prepare a water-blocking layer, the water-blocking layer is beeswax, paraffin and carnauba wax, of which 50% beeswax, 40% paraffin, and 10% carnauba wax. The operation steps are as follows: (1) Capsules are prepared by the positive drop method, the core layer is water, and the raw material of the capsule wall layer is sodium alginate solution; (2) The surface of the capsule is coated with a water-blocking layer, and the water-blocking layer is 50% beeswax, 40% paraffin %, carnauba wax 10%, the capsules were treated in the above mixed wax for 1min, and then solidified at low temperature; when preparing capsules, in order to ensure the fluidity of sodium alginate, the temperature was controlled at 60°C. In order to ensure the fluidity of the mixture, the temperature Controlled at 80°C.

Comparative example 3

A preparation method of a high-efficiency water-blocking and anti-penetration capsule, which is produced according to the following steps: preparing a core layer, the core layer is water; preparing a capsule wall layer, and the raw material of the capsule wall layer is sodium alginate solution with a concentration of 3%; the coagulation bath is chlorine Calcium solution, the concentration is 10%; prepare a water-blocking layer, the water-blocking layer is beeswax, paraffin and carnauba wax, wherein beeswax is 50%, paraffin wax is 40%, and carnauba wax is 10%. The outermost layer is calcium alginate. The operation steps are as follows: (1) Capsules are prepared by the positive drop method, the core layer is water, and the capsule wall layer is sodium alginate; (2) The surface of the capsule is covered with a water-blocking layer, and the water-blocking layer is 50% beeswax, 40% paraffin, 10% carnauba wax, treated in the above mixed wax at 50°C for 1min, and then solidified at low temperature; (3) soak the capsules prepared in step (2) in 5% sodium alginate solution for 10min, and then soak them in 1% calcium chloride The solution coagulated for 1h. When preparing the capsules, in order to ensure the fluidity of the sodium alginate, the temperature was controlled at 60°C, and in order to ensure the fluidity of the mixed wax, the temperature was controlled at 80°C.

The capsules in the above examples and comparative examples were tested to compare the performance of the capsules under different factors.

Capsule diameter

Take 10 capsules at random, use filter paper to dry the surface moisture, measure the maximum particle diameter D _max and the minimum particle diameter D _min of each capsule with an electronic digital caliper, record and calculate the average particle diameter D;

Sphericity SF

By measuring the diameter of the capsule, the sphericity was calculated.

The formula is: SF=(D _max -D _min )/(D _max +D _min ); the larger the sphericity, the rounder and more uniform the capsule.

strength

Adopt DWY-iii dripping pill quality comprehensive testing instrument to test; Since the capsule of the present invention can be used in the field of cigarettes, it is required that the capsule is easy to pinch and its strength is less than 20N.

Silica gel color test

Utilize the principle that silica gel changes color when exposed to water, test the anti-penetration performance of capsules, the specific test method is: randomly select 50 capsules, put them in a sample bottle, add 50 pieces of color-changing silica gel, seal, put the sample bottle with samples and color-changing silica gel Put it in a desiccator at 25°C, and observe the color change of the silica gel in the sample bottle at regular intervals. Measure the discoloration time to characterize the water seepage effect. The test time is 30 days, and observe whether there is discoloration within 30 days.

Permeability

Randomly select 20 capsules, place them in an open environment, and test their weight loss rate for 7 days and 30 days, which is the water permeability.

Table 1: Performance results of capsules

Example 13: Add the capsules prepared in Example 1 to a cigarette filter to prepare a cigarette filter containing popping beads.

Example 14: The capsule prepared in Example 12 was used as a capsule for medicine.

Embodiment 15: The capsules prepared in Embodiment 12 are used as food additives, as food capsules.

Claims (9)

1. The impermeable capsule 1. one kind efficiently blocks water, 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 cyst wall layer, and material includes polyurethane, epoxy resin, third The one or more of olefin(e) acid ester, isocyanates, the first water blocking layer can be chemically reacted with cyst wall layer, it is described efficiently block water it is anti- It permeates the capsule permeability rate of 7 days and is less than 4%, sphericity SF<0.07.
2. 2. a kind of as described in claim 1 impermeable capsule that efficiently blocks water, which is characterized in that capsule further includes the 4th layer, the Four layers are 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 paraffin, beeswax or babassu One or more in wax.
3. 3. a kind of as described in claim 1 impermeable capsule that efficiently blocks water, which is characterized in that first water blocking layer and/or Second water blocking layer further includes inorganic salts, and the inorganic salts are carbonate, the one or more in sulfate, silicate.
4. 4. a kind of as described in claim 1 impermeable capsule that efficiently blocks water, which is characterized in that first water blocking layer and/or Second water blocking layer further includes inorganic salts, and the inorganic salts are gypsum.
5. The impermeable capsule 5. a kind of such as claim 1-2 any one of them efficiently blocks water, which is characterized in that sandwich layer is water or contains Water component.
6. It is 6. a kind of as claim 1-2 any one of them efficiently blocks water impermeable capsule, which is characterized in that the cyst wall layer is One or more in alginate, cellulose derivative, gelatin, chitosan, polyethylene glycol, polyvinyl alcohol.
7. A kind of preparation method of impermeable capsule 7. such as claim 1-6 any one of them efficiently blocks water, it is characterised in that bag 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 One or more in biology, gelatin, chitosan, polyethylene glycol, polyvinyl alcohol；(2) capsule surface coats the first water blocking layer； (3) the impermeable capsule surface that efficiently blocks water being prepared in step (2) coats the second water blocking layer.
8. The preparation method of impermeable capsule 8. a kind of such as claim 7 any one of them efficiently blocks water, which is characterized in that described For dropping preparation method for anti-drop method, temperature when preparing capsule is 50-80 DEG C.
9. The application of impermeable capsule 9. a kind of such as claim 1-8 any one of them efficiently blocks water, it is characterised in that：By capsule For food, medicine, Field of Tobacco.