CN111019158B - Solid water and preparation method and application thereof - Google Patents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/04—Alginic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/12—Agar-agar; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/162—Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/205—Compounds containing groups, e.g. carbamates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3442—Heterocyclic compounds having nitrogen in the ring having two nitrogen atoms in the ring
- C08K5/3445—Five-membered rings
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Abstract
The invention discloses solid water and a preparation method and application thereof, wherein the solid water comprises the following components in percentage by mass: 5-10% of phase A, 1-5% of phase C, 1-5% of phase D and the balance of phase B; wherein the phase A is a mixture of low acyl gellan gum, glycerin and butylene glycol; phase B is a mixture of allantoin, methylparaben, sodium alginate and water; phase C is a mixture of bis (hydroxymethyl) imidazolidinyl urea (and) iodopropynyl butyl carbamate and instant agar; phase D is potassium chloride solution and CaCl 2 A mixture of solutions.
Description
Technical Field
The invention belongs to the technical field of solid water preparation, and particularly relates to solid water as well as a preparation method and application thereof.
Background
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The solid water is also called dry water, contains more than 90 percent of water, is an ecological environment-friendly product integrating microorganism and chemical technology, and has the physical characteristics of solid substances compared with common water, and does not flow or evaporate at normal temperature, ice at 0 ℃ or melt at 100 ℃. The appearance looks more like an elastic gel. Can be transported, used and stored by conventional means at normal temperature.
The solid water in the prior art is in a solid state and a gel state, but has soft texture, is not dense, and has poor processing and shaping effects. Generally, the food is placed by using a fixed-shape packaging bottle and other structures. And the storage is sealed for long-term storage, and the storage period is about 3 months. Under open conditions, the water in the solid water can be completely volatilized in 3 months, and the solid matters in the solid water are polysaccharide substances and are continuously degraded in the storage process. The texture of the solid water changes and its filling properties decrease, which can adversely affect the filled product.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention aims to provide solid water and a preparation method and application thereof. The solid water has good processing performance, high strength and good water retention performance.
In order to solve the technical problems, the technical scheme of the invention is as follows:
solid water comprises the following components in percentage by mass: 5-10% of phase A, 1-5% of phase C, 1-5% of phase D and the balance of phase B;
wherein the phase A is a mixture of low acyl gellan gum, glycerin and butylene glycol;
phase B is a mixture of allantoin, methylparaben, sodium alginate and water;
phase C is a mixture of bis (hydroxymethyl) imidazolidinyl urea, iodopropynyl butyl carbamate and instant agar;
d phase is potassium chloride solution and CaCl 2 A mixture of solutions.
Phase A is a thermoplastic fluid which is not reversible, and is used for plasticizing multiphase compatibility, and the phase A has the following functions:
low acyl gellan gum: the gel has excellent gel performance, can form high-transparency stable gel, is harder and more brittle compared with the gel formed by high acyl gellan gum, is more beneficial to processing and forming, and can still keep good physical state at the high temperature of more than 100 ℃.
Glycerol: the water-retaining agent is used for enhancing the water-retaining property of the solid phase; the glycerol can be perfectly compatible with other components, is cheap and easy to obtain, and is a good water-retaining agent.
Butanediol: the butanediol has small molecules, is easy to dissolve in water, can well adsorb water molecules, has super-strong moisturizing capability and certain bacteriostatic effect, and can generate a synergistic effect when being used together with glycerin; research shows that the butanediol has high safety and no irritation to oral mucosa, so that the butanediol-containing solid water can be applied to the preparation of solid water.
Phase B is a base liquid for thickening and homogenizing, and the phase B comprises the following components:
allantoin: an amphoteric compound with wide application can be combined with various substances to form a double salt, and has good compatibility with other components; the allantoin has the effects of hydrophily, water absorption and reduction of water dissipation, and compared with other humectants, the allantoin can form a lubricating film on the surface of an object so as to reduce the water dissipation; in addition, allantoin has certain antioxidation, good safety and no irritation.
Methyl hydroxybenzoate: the preservative is neutral, non-irritant and almost non-toxic, has good effects on mould and saccharomycetes, and can act together with other preservatives to achieve mutually complementary antibacterial effects.
Sodium alginate: a thickener; the sodium alginate is complexed with calcium ions to form irreversible gel which is insoluble in water but has good water absorption and can play a role in retaining and fixing water; compared with other gels, the reaction of sodium alginate and calcium ions can conveniently and accurately control the reaction process and the strength of formed gel; in addition, the sodium alginate is degradable, safe and environment-friendly, and the botanical source is reliable and stable.
Water: the components are fully dissolved as the base liquid to form a uniform and stable solution so as to be beneficial to the reaction.
The phase C is a solid and is used for supporting the integral form of solid water, and the phase C comprises the following components in part by weight:
quick dissolving agar: a gelling agent in a form that supports solid water as a solid after gel formation; compared with other gels, the gel formed by the instant agar has moderate hardness and strength, can be complementary with the gel formed by the gellan gum and the sodium alginate, can be well compatible with other components, is not easy to react with other components, and can improve the stability of the system.
Bis (hydroxymethyl) imidazolidinyl urea and iodopropynyl butyl carbamate: the two broad-spectrum antibacterial agents have a synergistic effect compared with other preservatives, and can have a low-dose and high-efficiency antibacterial effect in a solid C phase;
and the phase D is reaction liquid, performs complex reaction with gellan gum and sodium alginate, and solidifies and forms the rest of colloid, wherein the phase D comprises the following components:
potassium chloride solution: the ion complexing agent plays a role in ion complexing; the potassium chloride can efficiently react with the gellan gum, and the formed complex is obviously improved in strength compared with the complex before reaction.
CaCl 2 Solution: calcium alginate insoluble substances are formed after the calcium alginate is crosslinked with sodium alginate, and compared with other gels, the calcium alginate has excellent performances in the aspects of strength, toughness and water absorption; compared with other crosslinking agents such as zinc ions and magnesium ions, CaCl 2 The reaction between the solution and sodium alginate has high specificity, fast speed and high effect, and CaCl 2 The solution has high stability, can well coexist with other components in the phase D, and is an excellent crosslinking agent.
In some embodiments, the mass ratio of low acyl gellan gum, glycerin, and butylene glycol in the a phase is 1-1.5:1-2: 1-2. The three substances are mixed to obtain a liquid phase with better water retention, so that the phase A and other phases can react more fully; experiments prove that the low acyl gellan gum has the most ideal gel effect when the mass fraction is 1-1.5%, and the addition amounts of the glycerol and the butanediol are both more appropriate when the addition amounts are 1-2%.
In some embodiments, the mass ratio of allantoin, methylparaben, sodium alginate and water in the B phase is: 0.08-0.15:0.04-0.06:2-4:85-90.
Furthermore, in the phase B, the mass ratio of allantoin, methyl hydroxybenzoate, sodium alginate and water is as follows: 0.1:0.05:3:86.25.
In some embodiments, the mass ratio of bis (hydroxymethyl) imidazolidinyl urea to iodopropynyl butyl carbamate to quick dissolve agar in phase C is 0.2-0.3: 2.
In some embodiments, the weight percentage of the potassium chloride solution in the D phase is 8-12%, and CaCl is added 2 The mass percentage of the solution is 0.8-1.2%.
Further, potassium chloride solution and CaCl 2 The mass ratio of the solution is 2: 0.03-0.07.
The preparation method of the solid water comprises the following steps:
uniformly mixing the uniformly dispersed phase A and phase B, heating to 68-72 ℃, and preserving heat for 10-20 min; the operation can fully dissolve the components such as gellan gum, sodium alginate and the like but not cool the gel, and finally form a uniform and stable solution;
adding the phase C into the mixture of the phase A and the phase B, continuing to heat up, and preserving heat for a set time;
cooling the reaction system to 45-55 ℃, adding the phase D into the reaction system, stirring uniformly, and cooling; this step enables the four-phase components to be mixed and reacted thoroughly under suitable temperature conditions;
in some embodiments, the temperature after the temperature is continuously increased is 70-80 ℃, and the heat preservation time is 8-12 min.
The solid water is used as a filler in the preparation of cigarette filter sticks.
Because the cigarette smoke is dry in the smoking process, uncomfortable experience is caused to smokers. Solid water is used as a filler to fill the filter stick, and water volatilizes under the heating action of high-temperature smoke, so that a certain humidification effect on the high-temperature smoke can be achieved, and meanwhile, the filter stick cannot be soaked.
The invention has the beneficial effects that:
solid water is an effective way to entrap water. The moisture content of the solid water in the invention can reach more than 92 percent through the detection of a moisture tester; the water-proof paint has stable properties, the water loss is only about 20% after the paint is stored for 3 months in an open environment with the temperature of 25 ℃ and the relative humidity of 40-60%, the paint can be stored for 6 months in a normal-temperature closed environment without deterioration and the form is almost unchanged; the solid hydrogel strength can reach 300g/cm through testing 3 The composite filter stick has good processing performance, can be applied to a ternary cavity composite filter stick, can moisten smoke to a certain extent, and relieves discomfort such as dryness and throat.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The invention is further illustrated by the following examples:
example 1
Composition of solid water, as shown in table 1:
TABLE 1
The preparation method of the solid water comprises the following steps:
1) homogenizing and dispersing the phase A;
2) after the phase B is homogenized and dispersed, adding the phase A into the phase B, heating to 70 ℃, and keeping the temperature and stirring for 15 min;
3) adding phase C into phase (A + B), and stirring at 75 deg.C for 10 min;
4) cooling to 50 deg.C, adding phase D into the former phase, stirring for 1 min, cooling to 30 deg.C, and stirring.
The prepared solid water has the moisture content of about 92.7 percent and the solid content of about 7.3 percent; the water loss is only about 20 percent after the storage for 3 months in an open environment with the temperature of 25 ℃ and the relative humidity of 40 to 60 percent; the gel strength can reach 300g/cm 3 Has good processing performance, can be directly filled as a solid, and can also be added in a spray form.
Example 2
Composition of solid water, as shown in table 2:
TABLE 2
The preparation method of the solid water comprises the following steps:
1) homogenizing and dispersing the phase A;
2) after the phase B is homogenized and dispersed, adding the phase A into the phase B, heating to 68 ℃, and keeping the temperature and stirring for 20 min;
3) adding phase C into phase (A + B), and stirring at 80 deg.C for 10 min;
4) cooling to 55 deg.C, adding phase D into the front phase, stirring for 1 min, cooling to 30 deg.C, and stirring.
The prepared solid water has the moisture content of about 92.8 percent and the solid content of about 7.2 percent; at the temperature of 25 ℃ and the relative humidity of 40-60 percentIn an open environment, the water loss is only about 20 percent after 3 months of storage; the gel strength can reach 290g/cm 3 Has good processing performance, can be directly filled as a solid, and can also be added in a spray form.
Example 3
Composition of solid water, as shown in table 3:
TABLE 3
The preparation method of the solid water comprises the following steps:
1) homogenizing and dispersing the phase A;
2) after the phase B is homogenized and dispersed, adding the phase A into the phase B, heating to 72 ℃, and keeping the temperature and stirring for 15 min;
3) adding phase C into phase (A + B), and stirring at 70 deg.C for 10 min;
4) cooling to 55 deg.C, adding phase D into the front phase, stirring for 1 min, cooling to 30 deg.C, and stirring.
The prepared solid water has the moisture content of about 92.3 percent and the solid content of about 7.7 percent; the water loss is only about 20 percent after the storage for 3 months in an open environment with the temperature of 25 ℃ and the relative humidity of 40 to 60 percent; the gel strength can reach 300g/cm 3 Has good processing performance, can be directly filled as a solid, and can also be added in a spray form.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The application of solid water as a filler in the preparation of cigarette filter sticks is characterized in that: the solid water comprises the following components in percentage by mass: 5-10% of phase A, 1-5% of phase C, 1-5% of phase D and the balance of phase B;
wherein the phase A is a mixture of low-acyl gellan gum, glycerin and butanediol, and the mass ratio of the low-acyl gellan gum to the glycerin to the butanediol is 1-1.5:1-2: 1-2;
the phase B is a mixture of allantoin, methylparaben, sodium alginate and water, and the mass ratio of the allantoin to the methylparaben to the sodium alginate to the water is as follows: 0.08-0.15:0.04-0.06:2-4: 85-90;
the phase C is a mixture of bis (hydroxymethyl) imidazolidinyl urea, iodopropynyl butyl carbamate and instant agar, and the mass ratio of the sum of the mass of the bis (hydroxymethyl) imidazolidinyl urea and the iodopropynyl butyl carbamate to the mass of the instant agar is 0.2-0.3: 2;
phase D is potassium chloride solution and CaCl 2 A mixture of solutions;
the preparation method of the solid water comprises the following steps:
uniformly mixing the uniformly dispersed phase A and phase B, heating to 68-72 ℃, and preserving heat for 10-20 min;
adding the phase C into the mixture of the phase A and the phase B, continuing to heat up, and preserving heat for a set time;
and (3) cooling the reaction system to 45-55 ℃, adding the phase D into the reaction system, stirring uniformly, and cooling to obtain the product.
2. Use of solid water according to claim 1 as filler in the preparation of filter rods for cigarettes, characterized in that: in the phase B, the mass ratio of allantoin, methyl hydroxybenzoate, sodium alginate to water is as follows: 0.1:0.05:3:86.25.
3. Use of solid water according to claim 1 as filler in the preparation of filter rods for cigarettes, characterized in that: in the phase D, the mass percent of the potassium chloride solution is 8-12 percent, and CaCl is added 2 The mass percentage of the solution is 0.8-1.2%.
4. Use of solid water according to claim 1 as filler in the preparation of filter rods for cigarettes, characterized in that: potassium chloride solution and CaCl 2 The mass ratio of the solution is 2: 0.03-0.07.
5. Use of solid water according to claim 1 as filler in the preparation of filter rods for cigarettes, characterized in that: the temperature after the temperature rise is continuously 70-80 ℃, and the heat preservation time is 8-12 min.
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| CN101015559A (en) * | 2007-02-06 | 2007-08-15 | 复旦大学 | Instant gelling agent for treating allergic rhinitis |
| CN102078286A (en) * | 2009-11-26 | 2011-06-01 | 天津金耀集团有限公司 | In-situ gel containing ciclesonide for noses |
| CA2777428A1 (en) * | 2011-05-20 | 2012-11-20 | Nitto Denko Corporation | Edible jelly-form composition, jelly-form preparation and method for producing jelly-form preparation |
| CN103045360A (en) * | 2012-12-06 | 2013-04-17 | 深圳波顿香料有限公司 | Cigarette filter stick essence capsule, method for preparing same and cigarette |
| CN105342873A (en) * | 2015-11-02 | 2016-02-24 | 上海韵宜生物科技有限公司 | Novel skin care gel as well as preparation method and application thereof |
| CN105601950B (en) * | 2015-11-05 | 2018-03-23 | 湖北工业大学 | A kind of preparation method of the high-strength natural hydrogel material of sodium alginate agar dual network |
| CN105901764A (en) * | 2016-05-27 | 2016-08-31 | 阜阳卷烟材料厂 | Cigarette filter stick for improving cigarette smoking quality |
| CN109393555B (en) * | 2018-12-07 | 2021-03-26 | 云南巴菰生物科技有限公司 | Preparation method of cigarette capsule with processing resistance |
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