阅读说明：本技术 一种羟丙甲基纤维素和海藻多糖的填充空心胶囊制备方法 (Preparation method of filling hollow capsules of hydroxypropyl methylcellulose and algal polysaccharide ) 是由 王有平 于 2020-10-10 设计创作，主要内容包括：本发明公开了一种羟丙甲基纤维素和海藻多糖的填充空心胶囊制备方法,包括以下步骤：步骤S1：制备内薄衣：以1公斤原料计算称取丙酮：200-4000克；加入羟丙基甲基纤维素邻苯二甲酸酯：700-900克,搅拌；加入药用聚丙烯酸树脂Ⅱ：100-300克,搅拌；加入95％乙醇：200-400克,搅拌；加入聚乙二醇4000：50-150克；加入柠檬酸三乙酯：6.5-8.5克。本发明制备的羟丙甲纤维素空心充液空心胶囊可以填充水溶性液体或液态油状物,具有天然无污染、贮存期长、含水分少、不易吸潮、不易脆碎及崩解时限稳定、外观靓丽、透明度高、结构精美、各项指标及安全性居优等特点,且生产成本低,利润回报率高。(The invention discloses a preparation method of a filling hollow capsule of hydroxypropyl methylcellulose and algal polysaccharide, which comprises the following steps: step S1: preparing an inner thin coat: weighing acetone according to the weight ratio of 1 kg of raw materials: 200-4000 g; adding hydroxypropyl methylcellulose phthalate: 700 and 900 g, stirring; adding medicinal polyacrylic resin II: 100-300 g, stirring; adding 95% ethanol: 200 and 400 g, stirring; adding polyethylene glycol 4000: 50-150 g; adding triethyl citrate: 6.5-8.5 g. The hydroxypropyl methylcellulose hollow liquid-filled hollow capsule prepared by the invention can be filled with water-soluble liquid or liquid oily substances, has the characteristics of nature, no pollution, long storage period, less moisture content, difficult moisture absorption, difficult friability, stable disintegration time limit, beautiful appearance, high transparency, exquisite structure, excellent indexes and safety and the like, and is low in production cost and high in profit return rate.)

1. A preparation method of a filling hollow capsule of hydroxypropyl methylcellulose and algal polysaccharide is characterized by comprising the following steps:

step S1: preparing an inner thin coat: weighing acetone according to 1 kg of raw materials: 200-4000 g; adding hydroxypropyl methylcellulose phthalate: 700 and 900 g, stirring; adding medicinal polyacrylic resin II: 100-300 g, stirring; adding 95% ethanol: 200 and 400 g, stirring; adding polyethylene glycol 4000: 50-150 g, stirring; adding triethyl citrate: 6.5-8.5 g, stirring; adding glycerol or polyterpinol-80: 6.5-8.5 g, stirring; adding diethyl phthalate: 50-150 g, stirring;

step S2: carrying out sol on the hydroxypropyl methylcellulose hollow capsule raw material:

adding water: adding a proper amount of purified water into the sol tank according to the requirement of batch production instructions, wherein the weighing process needs to be accurate;

feeding, heating, feeding and stirring:

feeding tailings: according to the requirement of batch production instructions, adding metered purified water into a sol tank, starting a stirring motor, slowly adding weighed tailings into the sol tank, and starting to heat after stirring is stopped;

and (3) heating: setting the temperature controller at 95 ℃, starting a steam main valve, setting steam to be heated, and starting a steam electric control valve; steam enters through an upper interlayer pipeline of the sol tank, flows out through a lower interlayer pipeline, and is changed into condensed water through an output valve to be discharged; feeding raw materials and auxiliary materials and stirring: after the temperature of the gel liquid in the gel dissolving tank is heated to 95 ℃, slowly adding the weighed hydroxypropyl methylcellulose moderate carrageenan into the gel dissolving tank, and stirring for 20 minutes until the uniform stirring is realized; slowly adding the weighed auxiliary materials into a sol tank according to the requirement of a production order sheet, and uniformly stirring;

stirring at high temperature, vacuumizing, and dissolving: after all raw materials, auxiliary materials and tailings are fed according to a production instruction list, heating to 95 ℃ for sol, opening a vacuum pump valve switch, controlling the pressure to be 0.060-0.075MPa, and vacuumizing while stirring to remove bubbles; keeping the temperature of the glue solution in the glue dissolving tank at 95 ℃, stirring at high temperature for 60 minutes, and then cooling;

cooling and stirring: setting a sol filling temperature controller to be 50 ℃, setting a hot water tank temperature controller to cool hot water at 35 ℃, and when an electric control hot water valve is opened, circulating water for cooling flows from a lower interlayer pipeline of the glue pot to an upper interlayer pipeline of the glue pot through a hot water tank and then returns to the hot water tank to realize heat dissipation and cooling of the circulating water; adjusting the flow rate to slowly reduce the temperature of the glue solution to a specified temperature, and stirring while reducing the temperature to ensure that the glue solution is uniform;

stirring at constant temperature: when the temperature of the glue solution is reduced to 50 ℃, continuously stirring for 60 minutes at constant temperature to ensure that the glue solution is uniformly dispersed;

sixthly, viscosity measurement-correction-glue release: after stirring for 60 minutes at constant temperature, turning off the stirring motor, and stopping stirring;

keeping the temperature: respectively setting the body heat preservation temperature of 53 ℃ and the cap heat preservation temperature of 51 ℃ according to the actual temperature requirements of the glue solution of the upper body and the cap glue barrel of the production line, and detecting whether the actual temperature of the glue solution of the heat preservation barrel meets the actual temperature requirements of the glue solution of the upper body and the cap glue barrel of the production line every 2 hours by using a thermometer to ensure that the glue solution is placed for 18-24 hours for standby application;

step S3: preparing a capsule:

preparing:

adjusting the temperature and humidity of the three sections of glue dipping chambers, wherein the temperature of the glue dipping chamber of the inner thin coat is as follows: 22-24 ℃ and the relative humidity is 35-45%; front chamber temperature: 22.5 plus or minus 0.5 ℃ and relative humidity of 50-65 percent; rear chamber temperature: 31.5 ± 0.5 ℃, relative humidity: 30 to 45 percent;

operation II: simultaneously starting to put the inner thin-coat glue into the two sections of inner thin-coat glue tanks, keeping the inner thin-coat glue solution in the glue barrel at normal temperature without heating, stabilizing for 5-15 minutes after putting glue bundles for 30 minutes, and starting to dip the two sections of inner thin-coat glue after bubbles disappear; meanwhile, when the temperature of the front chamber glue dipping tank reaches a set temperature, glue is released, and the actual temperature of the glue solution of the glue barrel is 1.0 ℃ higher than that of the glue solution of the glue tank; then, glue discharging is started, the temperature of the glue tank is measured after the glue bundle is discharged for 30 minutes, and the actual temperature of the glue solution of the glue tank is adjusted according to the viscosity of the glue solution; starting an online viscometer to measure viscosity, controlling the viscosity of the cap glue solution at 2200 centipoises, controlling the viscosity of the body glue solution at 2300 centipoises, controlling the viscosity of the cap glue solution at 2300 centipoises, and starting to dip the hypromellose glue solution after the inner thin-coat mold circulates to the glue dipping front chamber after the viscosity is stabilized for 5-15 minutes; and adjusting the temperature of the rubber groove according to the wall thickness, and adjusting the position of the rubber groove according to the top thickness to ensure that the wall thickness and the top thickness meet the quality standard.

2. The method for preparing the filled hollow capsule of hydroxypropyl methylcellulose and algal polysaccharide according to claim 1, wherein in the step S1, the raw material ratio of the inner thin coating is as follows: 80% of hydroxypropyl methylcellulose phthalate and 20% of medicinal polyacrylic resin II.

3. The method of claim 1, wherein in step S1, the polyethylene glycol 4000 is stirred with 200 g of 95% ethanol, and then heated with 80 ℃ hot water to completely dissolve the polyethylene glycol 4000, and then cooled to obtain the hydroxypropyl methylcellulose and algal polysaccharide filled hollow capsule.

4. The method for preparing filled hollow capsules of hydroxypropylmethylcellulose and algal polysaccharide according to claim 1, wherein in said step S1, the technological parameters of said inner thin-coating require: preparing in sequence, stirring for 24 hours, and filtering with 200 meshes; filtering, and sealing for 24 hours for later use; when dipping the inner thin coat, adding alcohol dropwise to supplement the volatile loss; the time for dipping the thin underwear once is 7-9 seconds.

5. The method for preparing hydroxypropyl methylcellulose and algal polysaccharide filled hollow capsules according to claim 1, wherein in step S2, the auxiliary material is titanium dioxide mother liquor or pigment liquid.

6. The method of claim 1, wherein in step S2, the step of evacuating and debubbling comprises: when the liquid level rises to about 20cm away from the vacuum air suction port, half opening the exhaust valve to lower the liquid level; repeating the action for 4-5 times until the liquid level does not rise any more, closing the vacuum valve, and stopping vacuumizing.

7. The method of claim 1, wherein in step S2, the measuring, calibrating and releasing operations comprise: taking a proper amount of glue solution by using a 500ml beaker, placing the glue solution in a 50 ℃ constant temperature water bath, accurately measuring the viscosity value of the glue solution by using an online viscometer, controlling the time to be 10 minutes, wherein the viscosity value requirement meets 2300-2400cps, and if the viscosity value of the glue solution is not in a specified range, adding a certain proportion of 60 ℃ hot water and stirring for 30 minutes to perform viscosity correction until the viscosity value meets the requirement, and filling the original record; when the viscosity value correction of the glue solution meets the requirement, connecting a glue placing pipe, placing the glue placing pipe into a heat-insulated glue barrel, ensuring that the water level and the water temperature of an interlayer of the heat-insulated barrel meet the requirement, and starting to place the glue by opening a glue placing valve at the bottom of a glue dissolving tank; after the glue is put, the glue barrel is placed in a heat insulation area, a power supply and a sensor are plugged, and the body or cap glue solution state indication sheets are filled and written respectively.

8. The method of claim 1, wherein in step S3, the relative viscosity of the dip tank dope is as follows: 2200-2400cps, the inspection standard of the glue dipping tank is to inspect the circulating water temperature of the glue dipping tank every 2 hours, the temperature of the cap glue tank is controlled between 51-53 ℃, the temperature of the body glue tank is controlled between 50-52 ℃, the motor speed is as follows: 20-30 r/min.

Technical Field

The invention relates to the technical field of capsule preparation, in particular to a preparation method of a filling hollow capsule of hydroxypropyl methylcellulose and algal polysaccharide.

Background

With the increase of capsule varieties, the diversity of the contents of the capsules is gradually recognized, and the gelatin hollow capsules have the compatibility problem with some contents with special properties. For example, a content containing an aldehyde group or reacting under certain conditions to form an aldehyde group may cause a crosslinking reaction of gelatin; the content with strong reducibility can generate Maillard reaction with gelatin; the content with strong hygroscopicity can dehydrate the shell of the gelatin capsule and lose the original toughness. The stability problems of the above-mentioned gelatin hollow capsules have led to increased interest in the development of new capsule materials. Therefore, with the research and development and industrialization of plant-derived hollow capsules (pullulan hollow capsules, hypromellose hollow capsules and hydroxypropyl starch hollow capsules) in China, the plant-derived hollow capsules have the characteristics of unique safety, stability, antibacterial property, relevance, no obstacle, superiority, value increasing property, environmental protection, inertia and the like, make up the defects of animal-derived gelatin hollow capsules, solve the special requirement of capsule compatibility on hollow capsules and change the product structure of the medicinal hollow capsules to a certain extent. However, the prescription of the plant source capsule is complex, some gelling agents need to be added, and the production process is also complex. Compared with the plant source capsule, the animal source gelatin capsule has the advantages of absolute glossiness and fluency of the formed appearance, and can be absorbed by human body due to the fact that the main raw material of the gelatin capsule is the plateau protein gelatin besides the function of the carrier.

The capsule can be filled with powder, granules and part of solid oily substance, whether the capsule is a conventional gelatin capsule of animal origin or any plant capsule. The gelatin hollow capsule is filled with water-soluble liquid or liquid oily matter, the capsule can absorb water to swell, soften and deform, and the plant hollow capsule is filled with water-soluble liquid or liquid oily matter, and the capsule can be dissolved, so that the preparation method of the filling hollow capsule of hydroxypropyl methylcellulose and algal polysaccharide is provided for solving the problems.

Disclosure of Invention

Based on the technical problems in the background art, the invention provides a preparation method of a filling hollow capsule of hydroxypropyl methylcellulose and algal polysaccharide.

The invention provides a preparation method of a filling hollow capsule of hydroxypropyl methylcellulose and algal polysaccharide, which comprises the following steps:

step S1: preparing an inner thin coat: weighing acetone according to 1 kg of raw materials: 200-4000 g; adding hydroxypropyl methylcellulose phthalate: 700 and 900 g, stirring; adding medicinal polyacrylic resin II: 100-300 g, stirring; adding 95% ethanol: 200 and 400 g, stirring; adding polyethylene glycol 4000: 50-150 g, stirring; adding triethyl citrate: 6.5-8.5 g, stirring; adding glycerol or polyterpinol-80: 6.5-8.5 g, stirring; adding diethyl phthalate: 50-150 g, stirring;

step S2: carrying out sol on the hydroxypropyl methylcellulose hollow capsule raw material:

adding water: adding a proper amount of purified water into the sol tank according to the requirement of batch production instructions, wherein the weighing process needs to be accurate;

feeding, heating, feeding and stirring:

feeding tailings: according to the requirement of batch production instructions, adding metered purified water into a sol tank, starting a stirring motor, slowly adding weighed tailings into the sol tank, and starting to heat after stirring is stopped;

and (3) heating: setting the temperature controller at 95 ℃, starting a steam main valve, setting steam to be heated, and starting a steam electric control valve; steam enters through an upper interlayer pipeline of the sol tank, flows out through a lower interlayer pipeline, and is changed into condensed water through an output valve to be discharged; feeding raw materials and auxiliary materials and stirring: after the temperature of the gel liquid in the gel dissolving tank is heated to 95 ℃, slowly adding the weighed hydroxypropyl methylcellulose moderate carrageenan into the gel dissolving tank, and stirring for 20 minutes until the uniform stirring is realized; slowly adding the weighed auxiliary materials into a sol tank according to the requirement of a production order sheet, and uniformly stirring;

stirring at high temperature, vacuumizing, and dissolving: after all raw materials, auxiliary materials and tailings are fed according to a production instruction list, heating to 95 ℃ for sol, opening a vacuum pump valve switch, controlling the pressure to be 0.060-0.075MPa, and vacuumizing while stirring to remove bubbles; keeping the temperature of the glue solution in the glue dissolving tank at 95 ℃, stirring at high temperature for 60 minutes, and then cooling;

cooling and stirring: setting a sol filling temperature controller to be 50 ℃, setting a hot water tank temperature controller to cool hot water at 35 ℃, and when an electric control hot water valve is opened, circulating water for cooling flows from a lower interlayer pipeline of the glue pot to an upper interlayer pipeline of the glue pot through a hot water tank and then returns to the hot water tank to realize heat dissipation and cooling of the circulating water; adjusting the flow rate to slowly reduce the temperature of the glue solution to a specified temperature, and stirring while reducing the temperature to ensure that the glue solution is uniform;

stirring at constant temperature: when the temperature of the glue solution is reduced to 50 ℃, continuously stirring for 60 minutes at constant temperature to ensure that the glue solution is uniformly dispersed;

sixthly, viscosity measurement-correction-glue release: after stirring for 60 minutes at constant temperature, turning off the stirring motor, and stopping stirring;

keeping the temperature: respectively setting the body heat preservation temperature of 53 ℃ and the cap heat preservation temperature of 51 ℃ according to the actual temperature requirements of the glue solution of the upper body and the cap glue barrel of the production line, and detecting whether the actual temperature of the glue solution of the heat preservation barrel meets the actual temperature requirements of the glue solution of the upper body and the cap glue barrel of the production line every 2 hours by using a thermometer to ensure that the glue solution is placed for 18-24 hours for standby application;

step S3: preparing a capsule:

preparing:

adjusting the temperature and humidity of the three sections of glue dipping chambers, wherein the temperature of the glue dipping chamber of the inner thin coat is as follows: 22-24 ℃ and the relative humidity is 35-45%; front chamber temperature: 22.5 plus or minus 0.5 ℃ and relative humidity of 50-65 percent; rear chamber temperature: 31.5 ± 0.5 ℃, relative humidity: 30 to 45 percent;

operation II: simultaneously starting to put the inner thin-coat glue into the two sections of inner thin-coat glue tanks, keeping the inner thin-coat glue solution in the glue barrel at normal temperature without heating, stabilizing for 5-15 minutes after putting glue bundles for 30 minutes, and starting to dip the two sections of inner thin-coat glue after bubbles disappear; meanwhile, when the temperature of the front chamber glue dipping tank reaches a set temperature, glue is released, and the actual temperature of the glue solution of the glue barrel is 1.0 ℃ higher than that of the glue solution of the glue tank; then, glue discharging is started, the temperature of the glue tank is measured after the glue bundle is discharged for 30 minutes, and the actual temperature of the glue solution of the glue tank is adjusted according to the viscosity of the glue solution; starting an online viscometer to measure viscosity, controlling the viscosity of the cap glue solution at 2200 centipoises, controlling the viscosity of the body glue solution at 2300 centipoises, controlling the viscosity of the cap glue solution at 2300 centipoises, and starting to dip the hypromellose glue solution after the inner thin-coat mold circulates to the glue dipping front chamber after the viscosity is stabilized for 5-15 minutes; and adjusting the temperature of the rubber groove according to the wall thickness, and adjusting the position of the rubber groove according to the top thickness to ensure that the wall thickness and the top thickness meet the quality standard.

Preferably, in step S1, the raw material ratio of the inner thin coating is: 80% of hydroxypropyl methylcellulose phthalate and 20% of medicinal polyacrylic resin II.

Preferably, in step S1, the polyethylene glycol 4000 is prepared by stirring 200 g of 95% alcohol, heating with 80 ℃ hot water to completely dissolve the polyethylene glycol, and cooling, thereby improving the toughness.

Preferably, in step S1, the process parameters of the inner thin garment require: preparing in sequence, stirring for 24 hours, and filtering with 200 meshes; filtering, and sealing for 24 hours for later use; when dipping the inner thin coat, adding alcohol dropwise to supplement the volatile loss; the time for dipping the thin underwear once is 7-9 seconds.

Preferably, in step S2, the auxiliary material is titanium dioxide mother liquor or pigment liquor.

Preferably, in step S2, the vacuum-pumping and bubble-removing operation is: when the liquid level rises to about 20cm away from the vacuum air suction port, half opening the exhaust valve to lower the liquid level; repeating the action for 4-5 times until the liquid level does not rise any more, closing the vacuum valve, and stopping vacuumizing.

Preferably, in step S2, the measuring, correcting and glue releasing operations include: taking a proper amount of glue solution by using a 500ml beaker, placing the glue solution in a 50 ℃ constant temperature water bath, accurately measuring the viscosity value of the glue solution by using an online viscometer, controlling the time to be 10 minutes, wherein the viscosity value requirement meets 2300-2400cps, and if the viscosity value of the glue solution is not in a specified range, adding a certain proportion of 60 ℃ hot water and stirring for 30 minutes to perform viscosity correction until the viscosity value meets the requirement, and filling the original record; when the viscosity value correction of the glue solution meets the requirement, connecting a glue placing pipe, placing the glue placing pipe into a heat-insulated glue barrel, ensuring that the water level and the water temperature of an interlayer of the heat-insulated barrel meet the requirement, and starting to place the glue by opening a glue placing valve at the bottom of a glue dissolving tank; after the glue is put, the glue barrel is placed in a heat insulation area, a power supply and a sensor are plugged, and the body or cap glue solution state indication sheets are filled and written respectively.

Preferably, in step S3, the relative viscosity of the dipping glue tank glue solution is: 2200-2400cps, the inspection standard of the glue dipping tank is to inspect the circulating water temperature of the glue dipping tank every 2 hours, the temperature of the cap glue tank is controlled between 51-53 ℃, the temperature of the body glue tank is controlled between 50-52 ℃, the motor speed is as follows: 20-30 r/min.

The preparation method of the filling hollow capsule of hydroxypropyl methylcellulose and algal polysaccharide has the beneficial effects that:

(1) the hypromellose capsule is prepared by taking hypromellose as a main raw material and adding a certain proportion of algal polysaccharides, and the two raw materials have natural products, can meet the requirements of various religious and vegetarian diet habit crowds, and have high acceptance; the algal polysaccharide has the characteristics of high gel strength, high plasticity, good film forming performance, stable chemical performance and the like, and the polysaccharide component in the algal polysaccharide also has the effects of reducing blood fat, reducing blood sugar, resisting oxidation, resisting tumors and the like. Algal polysaccharide is an indispensable natural dietary fiber for human bodies, has unique nutrition, can combine organic matters, slow down the absorption of the human bodies to fatty sugar and bile salt, reduce cholesterol in serum and liver, inhibit the increase of total fat and total fatty acid concentration, reduce triglyceride and blood sugar in blood, improve the digestion and absorption of nutrient substances of the human bodies, and simultaneously can inhibit the accumulation and absorption of harmful elements such as radioactive strontium, cadmium, lead and the like in the human bodies in intestinal tracts. Has certain effect on preventing hypertension, coronary heart disease, obesity, diabetes and other modern diseases and intestinal tract system diseases. Has the functions of improving the immunity of human bodies, reducing blood fat and the like;

(2) the hydroxypropyl methylcellulose hollow capsule has unique inertia, is not influenced by the temperature and humidity of the environment, avoids the risk of influencing the quality in transportation and storage, and has the longest quality guarantee period; and because the capsule is made of plant fiber, the prepared capsule is not easy to become crisp. Completely avoids the trouble of some infectious disease sources possibly possessed by the animal hollow capsule, and is an ideal upgrade substitute for the traditional animal capsule. The hydroxypropyl methylcellulose hollow liquid-filled hollow capsule is a hollow capsule which can be filled with water-soluble liquid. Conventional gelatin capsules and plant empty capsules can only be filled with powder, granules and part of the oil. The hypromellose hollow liquid-filled hollow capsule is originated from one requirement of European hospitals, and the injection prepared by skin test injection is replaced by oral capsule (filled with water-soluble injection liquid).

The hydroxypropyl methylcellulose hollow liquid-filled hollow capsule prepared by the invention can be filled with water-soluble liquid or liquid oily substances, has the characteristics of nature, no pollution, long storage period, less moisture content, difficult moisture absorption, difficult friability, stable disintegration time limit, beautiful appearance, high transparency, exquisite structure, excellent indexes and safety and the like, and is low in production cost and high in profit return rate.

Drawings

Fig. 1 is a process flow diagram of a method for preparing filled hollow capsules of hydroxypropyl methylcellulose and algal polysaccharides according to the present invention.

Detailed Description

The present invention will be further illustrated with reference to the following specific examples.

Example one

A method for preparing a filled hollow capsule of hydroxypropyl methylcellulose and algal polysaccharide, as shown in fig. 1, comprising the following steps:

step S1: preparing an inner thin coat: weighing acetone according to 1 kg of raw materials: 2000 g; adding hydroxypropyl methylcellulose phthalate: 700 g, stirring; adding medicinal polyacrylic resin II: 175 g, stirring; adding 95% ethanol: 200 g, stirring; adding polyethylene glycol 4000: stirring 50 g; adding triethyl citrate: 6.5 g, stirring; adding glycerol or polyterpinol-80: 6.5 g, stirring; adding diethyl phthalate: stirring 50 g;

step S2: carrying out sol on the hydroxypropyl methylcellulose hollow capsule raw material:

adding water: adding a proper amount of purified water into the sol tank according to the requirement of batch production instructions, wherein the weighing process needs to be accurate;

feeding, heating, feeding and stirring:

feeding tailings: according to the requirement of batch production instructions, adding metered purified water into a sol tank, starting a stirring motor, slowly adding weighed tailings into the sol tank, and starting to heat after stirring is stopped;

and (3) heating: setting the temperature controller at 95 ℃, starting a steam main valve, setting steam to be heated, and starting a steam electric control valve; steam enters through an upper interlayer pipeline of the sol tank, flows out through a lower interlayer pipeline, and is changed into condensed water through an output valve to be discharged; feeding raw materials and auxiliary materials and stirring: after the temperature of the gel liquid in the gel dissolving tank is heated to 95 ℃, slowly adding the weighed hydroxypropyl methylcellulose moderate carrageenan into the gel dissolving tank, and stirring for 20 minutes until the uniform stirring is realized; slowly adding the weighed auxiliary materials into a sol tank according to the requirement of a production order sheet, and uniformly stirring;

stirring at high temperature, vacuumizing, and dissolving: after all raw materials, auxiliary materials and tailings are fed according to the production instruction list, heating to 95 ℃ for sol, opening a vacuum pump valve switch, controlling the pressure to be 0.060MPa, and vacuumizing while stirring to remove bubbles; keeping the temperature of the glue solution in the glue dissolving tank at 95 ℃, stirring at high temperature for 60 minutes, and then cooling;

cooling and stirring: setting a sol filling temperature controller to be 50 ℃, setting a hot water tank temperature controller to cool hot water at 35 ℃, and when an electric control hot water valve is opened, circulating water for cooling flows from a lower interlayer pipeline of the glue pot to an upper interlayer pipeline of the glue pot through a hot water tank and then returns to the hot water tank to realize heat dissipation and cooling of the circulating water; adjusting the flow rate to slowly reduce the temperature of the glue solution to a specified temperature, and stirring while reducing the temperature to ensure that the glue solution is uniform;

stirring at constant temperature: when the temperature of the glue solution is reduced to 50 ℃, continuously stirring for 60 minutes at constant temperature to ensure that the glue solution is uniformly dispersed;

sixthly, viscosity measurement-correction-glue release: after stirring for 60 minutes at constant temperature, turning off the stirring motor, and stopping stirring;

keeping the temperature: respectively setting the body heat preservation temperature of 53 ℃ and the cap heat preservation temperature of 51 ℃ according to the actual temperature requirements of the glue solution of the upper body and the cap glue barrel of the production line, and detecting whether the actual temperature of the glue solution of the heat preservation barrel meets the actual temperature requirements of the glue solution of the upper body and the cap glue barrel of the production line every 2 hours by using a thermometer to ensure that the glue solution is placed for 18 hours for standby application;

step S3: preparing a capsule:

preparing:

adjusting the temperature and humidity of the three sections of glue dipping chambers, wherein the temperature of the glue dipping chamber of the inner thin coat is as follows: at 22 ℃ and a relative humidity of 35%; front chamber temperature: relative humidity of 50% at 22 deg.C; rear chamber temperature: 31 ℃, relative humidity: 30 percent;

operation II: simultaneously starting to place inner thin-coat glue in the two sections of inner thin-coat glue tanks, keeping the inner thin-coat glue solution in the glue barrel at normal temperature without heating, stabilizing for 5 minutes after 30 minutes of glue bundle placement, and starting to dip the two sections of inner thin-coat glue after bubbles disappear; meanwhile, when the temperature of the front chamber glue dipping tank reaches a set temperature, glue is released, and the actual temperature of the glue solution of the glue barrel is 1.0 ℃ higher than that of the glue solution of the glue tank; then, glue discharging is started, the temperature of the glue tank is measured after the glue bundle is discharged for 30 minutes, and the actual temperature of the glue solution of the glue tank is adjusted according to the viscosity of the glue solution; starting an online viscometer to measure viscosity, controlling the viscosity of a cap glue solution at 2200 centipoise, controlling the viscosity of a body glue solution at 2300 centipoise, and starting to dip a hypromellose glue solution after an inner thin-coat die circulates to a glue dipping front chamber after the viscosity is stabilized for 5 minutes; and adjusting the temperature of the rubber groove according to the wall thickness, and adjusting the position of the rubber groove according to the top thickness to ensure that the wall thickness and the top thickness meet the quality standard.

In this embodiment, in step S1, the raw material ratio of the inner thin coat is: 80% of hydroxypropyl methylcellulose phthalate and 20% of medicinal polyacrylic resin II; in step S1, polyethylene glycol 4000 is stirred with 200 g of 95% alcohol, and then heated with 80 ℃ hot water to be completely dissolved and cooled to obtain the polyethylene glycol with improved toughness; in step S1, the requirements of the process parameters of the underwear are as follows: preparing in sequence, stirring for 24 hours, and filtering with 200 meshes; filtering, and sealing for 24 hours for later use; when dipping the inner thin coat, adding alcohol dropwise to supplement the volatile loss; 7 seconds are needed for dipping the thin underwear once; in step S2, the auxiliary material is titanium dioxide mother liquor or pigment liquor; in step S2, the evacuation and debubbling operation is: when the liquid level rises to about 20cm away from the vacuum air suction port, half opening the exhaust valve to lower the liquid level; the action is repeated for 4 times until the liquid level does not rise any more, the vacuum valve is closed, and the vacuumizing is stopped.

In this embodiment, in step S2, the operations of measuring, correcting, and releasing glue are as follows: taking a proper amount of glue solution by using a 500ml beaker, placing the glue solution in a 50 ℃ constant temperature water bath, accurately measuring the viscosity value of the glue solution by using an online viscometer, controlling the time to be 10 minutes, wherein the viscosity value requirement meets 2300cps, if the viscosity value of the glue solution is not in a specified range, adding a certain proportion of 60 ℃ hot water, stirring for 30 minutes, correcting the viscosity until the viscosity value meets the requirement, and filling the original record; when the viscosity value correction of the glue solution meets the requirement, connecting a glue placing pipe, placing the glue placing pipe into a heat-insulated glue barrel, ensuring that the water level and the water temperature of an interlayer of the heat-insulated barrel meet the requirement, and starting to place the glue by opening a glue placing valve at the bottom of a glue dissolving tank; after the glue is put, the glue barrel is placed in a heat insulation area, a power supply and a sensor are plugged, and the body or cap glue solution state indication sheets are filled and written respectively.

In this embodiment, in step S3, the relative viscosity of the glue solution in the glue dipping tank is: 2200cps, the inspection standard of the glue dipping tank is that the circulating water temperature of the glue dipping tank is inspected every 2 hours, the temperature of the cap glue tank is controlled between 51 ℃, the temperature of the body glue tank is controlled between 50 ℃, and the motor speed is as follows: 20 r/min.

Example two

A preparation method of a filling hollow capsule of hydroxypropyl methylcellulose and algal polysaccharide comprises the following steps:

step S1: preparing an inner thin coat: weighing acetone according to 1 kg of raw materials: 3000 g; adding hydroxypropyl methylcellulose phthalate: 800 and 900 g, stirring; adding medicinal polyacrylic resin II: 200 g, stirring; adding 95% ethanol: 300 g, stirring; adding polyethylene glycol 4000: stirring 100 g; adding triethyl citrate: 7 g, stirring; adding glycerol or polyterpinol-80: 7 g, stirring; adding diethyl phthalate: stirring 100 g;

step S2: carrying out sol on the hydroxypropyl methylcellulose hollow capsule raw material:

adding water: adding a proper amount of purified water into the sol tank according to the requirement of batch production instructions, wherein the weighing process needs to be accurate;

feeding, heating, feeding and stirring:

feeding tailings: according to the requirement of batch production instructions, adding metered purified water into a sol tank, starting a stirring motor, slowly adding weighed tailings into the sol tank, and starting to heat after stirring is stopped;

and (3) heating: setting the temperature controller at 95 ℃, starting a steam main valve, setting steam to be heated, and starting a steam electric control valve; steam enters through an upper interlayer pipeline of the sol tank, flows out through a lower interlayer pipeline, and is changed into condensed water through an output valve to be discharged; feeding raw materials and auxiliary materials and stirring: after the temperature of the gel liquid in the gel dissolving tank is heated to 95 ℃, slowly adding the weighed hydroxypropyl methylcellulose moderate carrageenan into the gel dissolving tank, and stirring for 20 minutes until the uniform stirring is realized; slowly adding the weighed auxiliary materials into a sol tank according to the requirement of a production order sheet, and uniformly stirring;

stirring at high temperature, vacuumizing, and dissolving: after all raw materials, auxiliary materials and tailings are fed according to the requirement of a production instruction list, heating to 95 ℃ for sol, opening a vacuum pump valve switch, controlling the pressure to be 0.07MPa, and vacuumizing while stirring to remove bubbles; keeping the temperature of the glue solution in the glue dissolving tank at 95 ℃, stirring at high temperature for 60 minutes, and then cooling;

cooling and stirring: setting a sol filling temperature controller to be 50 ℃, setting a hot water tank temperature controller to cool hot water at 35 ℃, and when an electric control hot water valve is opened, circulating water for cooling flows from a lower interlayer pipeline of the glue pot to an upper interlayer pipeline of the glue pot through a hot water tank and then returns to the hot water tank to realize heat dissipation and cooling of the circulating water; adjusting the flow rate to slowly reduce the temperature of the glue solution to a specified temperature, and stirring while reducing the temperature to ensure that the glue solution is uniform;

stirring at constant temperature: when the temperature of the glue solution is reduced to 50 ℃, continuously stirring for 60 minutes at constant temperature to ensure that the glue solution is uniformly dispersed;

sixthly, viscosity measurement-correction-glue release: after stirring for 60 minutes at constant temperature, turning off the stirring motor, and stopping stirring;

keeping the temperature: respectively setting the body heat preservation temperature of 53 ℃ and the cap heat preservation temperature of 51 ℃ according to the actual temperature requirements of the glue solution of the upper body and the cap glue barrel of the production line, and detecting whether the actual temperature of the glue solution of the heat preservation barrel meets the actual temperature requirements of the glue solution of the upper body and the cap glue barrel of the production line every 2 hours by using a thermometer to ensure that the glue solution is placed for 18-24 hours for standby application;

step S3: preparing a capsule:

preparing:

adjusting the temperature and humidity of the three sections of glue dipping chambers, wherein the temperature of the glue dipping chamber of the inner thin coat is as follows: at 23 ℃, the relative humidity is 40 percent; front chamber temperature: at 22.5 ℃ and relative humidity of 60 percent; rear chamber temperature: 31.5 ℃, relative humidity: 40 percent;

operation II: simultaneously starting to place inner thin-coat glue in the two sections of inner thin-coat glue tanks, keeping the inner thin-coat glue solution in the glue barrel at normal temperature without heating, stabilizing for 10 minutes after 30 minutes of glue bundle placement, and starting to dip the two sections of inner thin-coat glue after bubbles disappear; meanwhile, when the temperature of the front chamber glue dipping tank reaches a set temperature, glue is released, and the actual temperature of the glue solution of the glue barrel is 1.0 ℃ higher than that of the glue solution of the glue tank; then, glue discharging is started, the temperature of the glue tank is measured after the glue bundle is discharged for 30 minutes, and the actual temperature of the glue solution of the glue tank is adjusted according to the viscosity of the glue solution; starting an online viscometer to measure viscosity, controlling the viscosity of the cap glue solution at 2200 centipoises, controlling the viscosity of the body glue solution at 2350 centipoises, and starting to dip the hydroxypropyl methylcellulose glue solution after the inner thin-coat mold circulates to the glue dipping front chamber after the viscosity is stabilized for 10 minutes; and adjusting the temperature of the rubber groove according to the wall thickness, and adjusting the position of the rubber groove according to the top thickness to ensure that the wall thickness and the top thickness meet the quality standard.

In this embodiment, in step S1, the raw material ratio of the inner thin coat is: 80% of hydroxypropyl methylcellulose phthalate and 20% of medicinal polyacrylic resin II; in step S1, polyethylene glycol 4000 is stirred with 200 g of 95% alcohol, and then heated with 80 ℃ hot water to be completely dissolved and cooled to obtain the polyethylene glycol with improved toughness; in step S1, the requirements of the process parameters of the underwear are as follows: preparing in sequence, stirring for 24 hours, and filtering with 200 meshes; filtering, and sealing for 24 hours for later use; when dipping the inner thin coat, adding alcohol dropwise to supplement the volatile loss; 8 seconds are needed for dipping the thin underwear once; in step S2, the auxiliary material is titanium dioxide mother liquor or pigment liquor; in step S2, the evacuation and debubbling operation is: when the liquid level rises to about 20cm away from the vacuum air suction port, half opening the exhaust valve to lower the liquid level; the action is repeated for 4 times until the liquid level does not rise any more, the vacuum valve is closed, and the vacuumizing is stopped.

In this embodiment, in step S2, the operations of measuring, correcting, and releasing glue are as follows: taking a proper amount of glue solution by using a 500ml beaker, placing the glue solution in a 50 ℃ constant temperature water bath pan, accurately measuring the viscosity value of the glue solution by using an online viscometer, controlling the time to be 10 minutes, wherein the requirement of the viscosity value meets 2350cps, and if the viscosity value of the glue solution is not in a specified range, adding a certain proportion of 60 ℃ hot water, stirring for 30 minutes to correct the viscosity until the viscosity value meets the requirement, and filling the original record; when the viscosity value correction of the glue solution meets the requirement, connecting a glue placing pipe, placing the glue placing pipe into a heat-insulated glue barrel, ensuring that the water level and the water temperature of an interlayer of the heat-insulated barrel meet the requirement, and starting to place the glue by opening a glue placing valve at the bottom of a glue dissolving tank; after the glue is put, the glue barrel is placed in a heat insulation area, a power supply and a sensor are plugged, and the body or cap glue solution state indication sheets are filled and written respectively.

In this embodiment, in step S3, the relative viscosity of the glue solution in the glue dipping tank is: 2300cps, the inspection standard of the glue dipping tank is to inspect the circulating water temperature of the glue dipping tank every 2 hours, the temperature of the cap glue tank is controlled between 52 ℃, the temperature of the body glue tank is controlled between 51 ℃, and the motor speed is as follows: 25 r/min.

EXAMPLE III

A preparation method of a filling hollow capsule of hydroxypropyl methylcellulose and algal polysaccharide comprises the following steps:

step S1: preparing an inner thin coat: weighing acetone according to 1 kg of raw materials: 4000 g; adding hydroxypropyl methylcellulose phthalate: 900 g, stirring; adding medicinal polyacrylic resin II: 225 g, stirring; adding 95% ethanol: 400 g, stirring; adding polyethylene glycol 4000: 150 g, stirring; adding triethyl citrate: 8.5 g, stirring; adding glycerol or polyterpinol-80: 8.5 g, stirring; adding diethyl phthalate: 150 g, stirring;

step S2: carrying out sol on the hydroxypropyl methylcellulose hollow capsule raw material:

adding water: adding a proper amount of purified water into the sol tank according to the requirement of batch production instructions, wherein the weighing process needs to be accurate;

feeding, heating, feeding and stirring:

feeding tailings: according to the requirement of batch production instructions, adding metered purified water into a sol tank, starting a stirring motor, slowly adding weighed tailings into the sol tank, and starting to heat after stirring is stopped;

and (3) heating: setting the temperature controller at 95 ℃, starting a steam main valve, setting steam to be heated, and starting a steam electric control valve; steam enters through an upper interlayer pipeline of the sol tank, flows out through a lower interlayer pipeline, and is changed into condensed water through an output valve to be discharged; feeding raw materials and auxiliary materials and stirring: after the temperature of the gel liquid in the gel dissolving tank is heated to 95 ℃, slowly adding the weighed hydroxypropyl methylcellulose moderate carrageenan into the gel dissolving tank, and stirring for 20 minutes until the uniform stirring is realized; slowly adding the weighed auxiliary materials into a sol tank according to the requirement of a production order sheet, and uniformly stirring;

stirring at high temperature, vacuumizing, and dissolving: after all raw materials, auxiliary materials and tailings are fed according to a production instruction list, heating to 95 ℃ for sol, opening a vacuum pump valve switch, controlling the pressure to be 0.075MPa, and vacuumizing while stirring to remove bubbles; keeping the temperature of the glue solution in the glue dissolving tank at 95 ℃, stirring at high temperature for 60 minutes, and then cooling;

cooling and stirring: setting a sol filling temperature controller to be 50 ℃, setting a hot water tank temperature controller to cool hot water at 35 ℃, and when an electric control hot water valve is opened, circulating water for cooling flows from a lower interlayer pipeline of the glue pot to an upper interlayer pipeline of the glue pot through a hot water tank and then returns to the hot water tank to realize heat dissipation and cooling of the circulating water; adjusting the flow rate to slowly reduce the temperature of the glue solution to a specified temperature, and stirring while reducing the temperature to ensure that the glue solution is uniform;

stirring at constant temperature: when the temperature of the glue solution is reduced to 50 ℃, continuously stirring for 60 minutes at constant temperature to ensure that the glue solution is uniformly dispersed;

sixthly, viscosity measurement-correction-glue release: after stirring for 60 minutes at constant temperature, turning off the stirring motor, and stopping stirring;

keeping the temperature: respectively setting the body heat preservation temperature of 53 ℃ and the cap heat preservation temperature of 51 ℃ according to the actual temperature requirements of the glue solution of the upper body and the cap glue barrel of the production line, and detecting whether the actual temperature of the glue solution of the heat preservation barrel meets the actual temperature requirements of the glue solution of the upper body and the cap glue barrel of the production line every 2 hours by using a thermometer to ensure that the glue solution is placed for 24 hours for standby;

step S3: preparing a capsule:

preparing:

adjusting the temperature and humidity of the three sections of glue dipping chambers, wherein the temperature of the glue dipping chamber of the inner thin coat is as follows: relative humidity of 45% at 24 ℃; front chamber temperature: relative humidity of 65% at 23 deg.C; rear chamber temperature: 32 ℃, relative humidity: 45 percent;

operation II: simultaneously starting to place inner thin-coat glue in the two sections of inner thin-coat glue tanks, keeping the inner thin-coat glue solution in the glue barrel at normal temperature without heating, stabilizing for 15 minutes after 30 minutes of glue bundle placement, and starting to dip the two sections of inner thin-coat glue after bubbles disappear; meanwhile, when the temperature of the front chamber glue dipping tank reaches a set temperature, glue is released, and the actual temperature of the glue solution of the glue barrel is 1.0 ℃ higher than that of the glue solution of the glue tank; then, glue discharging is started, the temperature of the glue tank is measured after the glue bundle is discharged for 30 minutes, and the actual temperature of the glue solution of the glue tank is adjusted according to the viscosity of the glue solution; starting an online viscometer to measure viscosity, controlling the viscosity of the cap glue solution at 2300 centipoise, controlling the viscosity of the body glue solution at 2400 centipoise, and starting to dip the hypromellose glue solution after the inner thin-coat die circulates to a glue dipping front chamber after the viscosity is stabilized for 15 minutes; and adjusting the temperature of the rubber groove according to the wall thickness, and adjusting the position of the rubber groove according to the top thickness to ensure that the wall thickness and the top thickness meet the quality standard.

In this embodiment, in step S1, the raw material ratio of the inner thin coat is: 80% of hydroxypropyl methylcellulose phthalate and 20% of medicinal polyacrylic resin II; in step S1, polyethylene glycol 4000 is stirred with 200 g of 95% alcohol, and then heated with 80 ℃ hot water to be completely dissolved and cooled to obtain the polyethylene glycol with improved toughness; in step S1, the requirements of the process parameters of the underwear are as follows: preparing in sequence, stirring for 24 hours, and filtering with 200 meshes; filtering, and sealing for 24 hours for later use; when dipping the inner thin coat, adding alcohol dropwise to supplement the volatile loss; dipping the thin underwear for 9 seconds; in step S2, the auxiliary material is titanium dioxide mother liquor or pigment liquor; in step S2, the evacuation and debubbling operation is: when the liquid level rises to about 20cm away from the vacuum air suction port, half opening the exhaust valve to lower the liquid level; this action was repeated 5 times until the liquid level did not rise any more, the vacuum valve was closed, and the evacuation was stopped.

In this embodiment, in step S2, the operations of measuring, correcting, and releasing glue are as follows: taking a proper amount of glue solution by using a 500ml beaker, placing the glue solution in a 50 ℃ constant temperature water bath, accurately measuring the viscosity value of the glue solution by using an online viscometer, controlling the time to be 10 minutes, wherein the viscosity value requirement meets 2400cps, if the viscosity value of the glue solution is not in a specified range, adding a certain proportion of 60 ℃ hot water, stirring for 30 minutes, correcting the viscosity until the viscosity value meets the requirement, and filling the original record; when the viscosity value correction of the glue solution meets the requirement, connecting a glue placing pipe, placing the glue placing pipe into a heat-insulated glue barrel, ensuring that the water level and the water temperature of an interlayer of the heat-insulated barrel meet the requirement, and starting to place the glue by opening a glue placing valve at the bottom of a glue dissolving tank; after the glue is put, the glue barrel is placed in a heat insulation area, a power supply and a sensor are plugged, and the body or cap glue solution state indication sheets are filled and written respectively.

In this embodiment, in step S3, the relative viscosity of the glue solution in the glue dipping tank is: 2400cps, the inspection standard of the glue dipping tank is to inspect the circulating water temperature of the glue dipping tank every 2 hours, the temperature of the cap glue tank is controlled to be 53 ℃, the temperature of the body glue tank is controlled to be 52 ℃, and the motor speed is as follows: 30 r/min.

All the performance tests of the hollow capsules manufactured in the above embodiments are passed, and the results are recorded as follows:

examples	Length deviation (millimeter) of A cap and B body	Storage period (sky)	Peculiar smell
				Example one	0.30	1470	Is free of
Example two	0.36	1468	Is free of
				EXAMPLE III	0.14	1482	Is free of

The empty capsule prepared by the invention can be filled with water-soluble liquid or liquid oily substance, has the characteristics of naturalness, no pollution, long storage period, less moisture content, difficult moisture absorption, difficult friability, stable disintegration time limit, beautiful appearance, high transparency, exquisite structure, various indexes, excellent safety and the like, and is low in production cost and high in profit return rate, and the third embodiment is the best embodiment.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.