CN105800719B - The preparation method and its purposes in tobacco of a kind of small-micelle water - Google Patents
The preparation method and its purposes in tobacco of a kind of small-micelle water Download PDFInfo
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- CN105800719B CN105800719B CN201610316880.2A CN201610316880A CN105800719B CN 105800719 B CN105800719 B CN 105800719B CN 201610316880 A CN201610316880 A CN 201610316880A CN 105800719 B CN105800719 B CN 105800719B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/22—Treatment of water, waste water, or sewage by freezing
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
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Abstract
The present invention discloses a kind of preparation method of small-micelle water method includes the following steps: (1) cools down pure water at room temperature with the rate of 0.5 DEG C/min, and when reaching each critical point, holding 30~60min of temperature then proceedes to cool down；When reaching 0 DEG C, 30~60min of temperature is kept；Then again with the cooling of 0.2 DEG C/min rate, when reaching each critical point, 30~60min of temperature is kept；Continue to cool down, when temperature reaches -6 DEG C, keeps 30~60min of temperature, obtain solid ice；(2) solid ice for obtaining step (1), is heated up with the rate of 0.2 DEG C/min, after the heating-up time is 120~210min, then is heated up with 0.5 DEG C/min rate, is reached after room temperature to get to the small-micelle water.
Description
Technical field
The present invention relates to a kind of purified water and preparation method and purposes, in particular to the preparation method of small-micelle water and its
Purposes in tobacco.
Background technique
Water, as the necessity of life, along with the increasingly raising of people's living standard, be sent to higher expectation and
It is required that.Water in nature be in the form of molecular structure existing for.Hydrone will form biggish point under the action of hydrogen bond
Son group, and biggish micel is unfavorable for absorption of the human body to water.The micel of water is smaller, and the penetration of water is stronger, is easier to
Into cell membrane, nutriment is transported, takes the rubbish of cell out of.
Water is made of two hydrogen atoms and an oxygen atom, the two hydrogen atoms are not in 180 degree and oxygen atom line
Property be coupled, but in V-shape be distributed.The constitution element and molecular structure of water make it with many unique properties, especially
It is the formation of hydrogen bond.It there are two the receptor that can produce hydrogen bond and generates hydrogen bond respectively in its structure and gives body, pass through between hydrone
The formation of hydrogen bond and generate different water-bounds, such as be similar to ice tetrahedron, dimer and polymer.
Hydrogen bond is a kind of slightly stronger than intermolecular force (Van der Waals force), many phase interactions weaker than covalent bond and ionic bond
With stability is weaker than covalent bond and ionic bond.In liquid water, one is incorporated in by stronger hydrogen bond action between several hydrones
It rises, i.e. generation molecular association, forms (H2O) the molecular cluster of n.Between hydrone hydrogen bond average bond energy be 21kJ/mol, when temperature,
Pressure change or by external force, provides the hydrogen bond between additional energy damages hydrone, and the chemical bond in hydrone not by
It destroys, the less small-micelle water of cluster number can be obtained.Hydrogen bond dissociation energy is 110kJ/mol, and being good for can be neither big nor small, is held very much
Easily connection is also easy to be broken.So the cluster structure of water clusters is always among continuous variation.
Research has shown that, by external energy, realizes the change of water molecule cluster number, such as at magnetic field facture, electric field
Logos, microwave treatment method, tourmaline facture, these methods produce small-micelle water, the subset water stability of preparation
Difference is restored to macromolecular mass tufted state again after a long time placement, and these methods can not continuity operates, production efficiency is low, warp
Ji property is poor, and time-consuming for preparation.
Summary of the invention
It is an object of the invention to it is poor for stability existing for existing technical solution, can not continuity operation, economy
Property it is poor the problems such as, provide a kind of new small-micelle water preparation method.
First aspect present invention is related to a kind of preparation method of small-micelle water, method includes the following steps:
(1) pure water at room temperature is cooled down with the rate of 0.5 DEG C/min, when reaching each critical point, is kept
30~60min of temperature then proceedes to cool down；When reaching 0 DEG C, 30~60min of temperature is kept；Then again with 0.2 DEG C/min
Rate cooling keeps 30~60min of temperature when reaching each critical point；Continue to cool down, when temperature reaches -6 DEG C, keep
30~60min of temperature, obtains solid ice；
(2) solid ice for obtaining step (1), is heated up with the rate of 0.2 DEG C/min, the heating-up time be 120~
It after 210min, then is heated up with 0.5 DEG C/min rate, is reached after room temperature to get to the small-micelle water.
Preferably, the critical point is 10 DEG C, 5 DEG C, 2 DEG C, 0 DEG C, -2 DEG C, -5 DEG C, -6 DEG C；The room temperature is 20~25
℃。
Second aspect of the present invention is related to small-micelle water prepared by the preparation method of the small-micelle water for improving
Permeability from amino acid to tobacco purposes.
Beneficial effects of the present invention:
1, the preparation method is that making water molecule cluster by energy exchange caused by ice-out Cheng Shui after freezing
Kinetic energy increase, the amplitude in equilbrium position also increases with it, thus in cluster structure chemical bond occur it is a degree of curved
Song, the change of the O-H key angular separation of the center line and its some molecule of adjacent hydrone, it will the fracture for leading to hydrogen bond has
Effect simplifies preparation method, is directly changed the structure of water molecule cluster, and having can continuity operation, formation efficiency height, economy
The advantages such as good.
2, preparation method of the invention, which is realized, is refined into small molecule cluster, water sample for the macromolecular cluster of water17O NMR half-peak
Wide numerical value is low, and the hydrogen-free linkage content of Raman spectrum is high, and stability is good, and solvability is high, can be preferably in agricultural, industrial aspect application
It promotes.
3, small-micelle water of the present invention improves a lot to the permeability of amino acid, is molten well in tobacco processing
Agent, the mouthfeel in tobacco, being conducive to tobacco finished product are promoted.
Detailed description of the invention
Fig. 1 is the specific embodiment schematic diagram of the method for the present invention.
Fig. 2 is the method for the present invention and other water samples17O liquid core magnetic value；Wherein A is Yunnan Zhong Yan company water sample, B is certain
Company's water sample, C are certain commercially available brand water sample, D is that water sample is made in the embodiment of the present invention 1, E is distillation water sample (blank water sample).
Fig. 3 is that water sample is made in subset water sample made from the method for the present invention and other methods17O liquid core magnetic value；1 is
Tourmaline method processing water sample, 2 be Magnitizing method processing water sample, 3 be electrolytic method processing water sample, 4 be the present invention in fact
Apply water sample made from example 1,5 for distillation water sample (blank water sample).
Fig. 4 is cigarette water sample in Yunnan, certain commercially available brand water sample, subset water sample of the invention and distillation water sample (blank
Water sample) Raman swarming spectrogram；
Specific embodiment
As shown in Figure 1, be a kind of device for preparing small-micelle water using Refrigeration Technique, the device include glass container 1,
Glass container interlayer 5, water inlet pipe 3, outlet pipe 4, refrigeration system 2, the interior refrigeration system 2 includes control cabinet, circulating pump, refrigeration
Equipment, refrigeration system 2 and water inlet pipe 3, glass container interlayer 5, outlet pipe 4 connect into a circulator；The glass container 1
It is a closed system, is the second constant temperature field artificially established, is packed into raw water source in glass container 1；System in refrigeration system 2
Cryogen flows into glass container interlayer 5 by water inlet pipe 3 and outflows back in refrigeration system 2 from outlet pipe 4.
The Raman spectrum for preparing small-micelle water of the method for the present invention offer,17The characteristics such as O-NMR liquid core magnetic value,
In17What O-NMR liquid core magnetic value was selected is this index of half-peak breadth.
Liquid nuclear-magnetism is the conventional means as performance molecular cluster size, due to liquid water itself particularity,17O-
H NMR spectroscopy line spectral line width in all Isotopes spectral lines is most narrow, therefore should select when being studied using nuclear magnetic resonance liquid water
With17O core measures.Since transverse relaxation process is the exchange of spin states between neighbouring core, and the cluster structure of water is bigger,
Spin states exchange faster between oxygen core and neighbouring core, and it is shorter that sample is restored to the time required for equilibrium state, spectral line
It is wider, therefore, it can reflect the average relative size of liquid water cluster structure using the width of Nmr Lines, spectral line is got over
Width, cluster are bigger；Spectral line is narrower, and cluster is smaller.17O-NMR half-peak breadth can be used for representing the characteristic of small-micelle water of the invention.
Raman spectrum is usually used in studying the performance of hydrone active force, Raman shift about 2600-4000cm-1Representative is water
The signal of this range can be separated five bands (band), different water samples by Gaussian function swarming by the OH stretching vibration of molecule
Principle when swarming is, the position of five bands is fixed, using each water sample half-breadth high level all, center position is divided
It is not about 3018, about 3223, about 3393, about 3506 and about 3624cm-1, first three position contributed by the strong hydrogen bonding between hydrone,
Both be afterwards mainly respectively weak hydrogen bond and the composition without hydrogen bond, the integral area of both rear band divided by five bands area summation
Value is defined as the percentage composition of hydrogen-free stroke degree (no hydrogen bond force strength) representative in measured hydrone.One
As for, the hydrogen-free stroke degree of deionized water is 21.29%.When hydrogen bond is destroyed, shown in Raman spectrum, strong hydrogen bonding
Band strength (area) reduces, and instead rises for weak hydrogen bond and the band strength without hydrogen bond, therefore, Raman spectrum can be used for generation
The characteristic of table small-micelle water of the invention.
Following instance is to further detailed analysis of the invention, and embodiments of the present invention are not limited thereto.
Embodiment 1: the preparation of small-micelle water of the present invention
By in 1 glass container 1 of water sample load map of Yunnan Zhong Yan company, refrigerant is packed into refrigeration system 2, adjusts control cabinet
The temperature program of refrigeration equipment, control cabinet adjust the temperature program of refrigeration equipment, and control sink rate of temperature fall is 0.5 DEG C/min,
When cooling to each critical point (10 DEG C, 5 DEG C, 2 DEG C, 0 DEG C), control temperature stablize 30-60min, after continue to cool down, be cooled to out
When existing trash ice (at 0 DEG C), then controlling rate of temperature fall is 0.2 DEG C/min, continues to be cooled to critical point (- 2 DEG C, -5 DEG C, -6 DEG C),
It controls temperature and stablizes 30-60min, when liquid becomes solid in glass container, stop cooling, when raw water source freezing is solid
When, then controlling sink heating rate is 0.2 DEG C/min, after the 120~210min that heats up, then adjusting heating rate is 0.5 DEG C/min
It is warmed to room temperature, the small-micelle water with small molecule clustering properties is obtained in glass container.
Embodiment 2: the liquid nuclear-magnetism of small-micelle water and other water samples of the present invention
Water sample is made in Yunnan Zhong Yan company water sample (A), certain company's water sample (B), certain commercially available brand water sample (C), embodiment 1
(D), blank water sample (E) carries out17O magnetic resonance detection is respectively charged into A, B, C, D, E water sample in nuclear magnetic tube, with liquid nuclear-magnetism
The instrument (Liquid Nuclear Magnetic Resonance, model AVANCE III are purchased from Brooker) that resonates is detected,
Nuclear magnetic tube is put into Nuclear Magnetic Resonance, is scanned 516 times, is obtained the width of Nmr Lines by the free quantum signal of O core,
And then available half-value width.
According to nuclear-magnetism result it is known that embodiment 1 has been successfully prepared small-micelle water.Yunnan Zhong Yan company water sample
(A) nuclear-magnetism value is 68.1Hz, and it is 48.6Hz that water sample (D), which is made, in embodiment 1, and half-value width has apparent reduction, illustrates small point
Sub- cluster is smaller (referring to attached drawing 2).
Embodiment 3: watery liquid nuclear-magnetism value ratio is made in the small-micelle water of the method for the present invention preparation and other inventive methods
Compared with
The water sample that the water sample (1) of tourmaline method processing, the water sample (2) of Magnitizing method processing, electrolytic method are handled
(3), water sample (4) made from embodiment 1 and blank group water sample (5) carry out17O magnetic resonance detection distinguishes 1,2,3,4,5 water samples
It is fitted into nuclear magnetic tube, with Liquid NMR instrument (Liquid Nuclear Magnetic Resonance, model AVANCE
III, it is purchased from Brooker) detected, nuclear magnetic tube is put into Nuclear Magnetic Resonance, is scanned 516 times, is interrogated by the free quantum of O core
Number obtain the width of Nmr Lines, and then available half-value width.
According to nuclear-magnetism result it is known that its half-value width of water sample made from the embodiment of the present invention 1 is minimum (48.6Hz),
It is exactly that the method for embodiment 1 can obtain the smaller water of molecular cluster (with reference to the column 4 of attached drawing 3).
Embodiment 4: the Raman spectrum of small-micelle water and other water samples of the present invention
Small-micelle water made from Yunnan Zhong Yan company water sample (A), certain commercially available brand water sample (B), the embodiment of the present invention 1
Sample (C), blank water sample (distilled water) (D) carry out Raman spectrum analysis, water sample drop on glass slide, wherein cover on glass slide
There is the rectangular silver strip of 0.1mm thickness, with laser Raman spectrometer (Laser Raman Spectrometer, model inVia
Reflex is purchased from thunder Manny) it is detected, the glass slide for being loaded with water sample is put under the microscope, with 532 nanometers of laser of wavelength
In measuring range 2800-3800cm-1In, each time for exposure is 30 seconds, after scanning 1 time, obtains OH stretching vibration signal and goes forward side by side
The analysis of row data swarming.Different water sample Raman spectrum swarming figures are shown in Fig. 4.
OH stretching vibration signal swarming position is set in 3018cm by the analysis of spectroscopic data swarming-1、3223cm-1、3393cm-1、3506cm-1And 3624cm-1, and when each sample swarming, using each water sample band half-breadth high level all.Wherein position
In 3506cm-1And 3624cm-1It is belonging respectively to the area of weak hydrogen bond and the composition band without hydrogen bond, with whole OH stretching vibration band
Area ratio is defined as hydrogen-free stroke degree.Raman spectroscopy measurement is as a result, as shown in table 1.
Table 1: the Raman light spectrum of different water samples
It is found that the hydrogen-free stroke degree highest of water sample (C) is made in the embodiment of the present invention 1 from table, reach 34.18%, it is right
According to the 12.53% of blank water sample (distilled water), obvious the method for the present invention has successfully prepared small-micelle water.
Embodiment 5: small-micelle water osmotic effect of the present invention
Amino acid is that the important substance of one kind in tobacco has significant contribution in terms of tobacco leaf fragrance quality, is synthetic proteins matter
With the raw material of nicotine, suitable amino acid helps to improve flue gas strength and increases richness in tobacco.On the one hand, amino acid fires
Burn the nitrogenous compound such as NH that can have an impact flue gas mass3；On the other hand, flue-cured tobacco dissociates during modulation, alcoholization and fermentation
Amino acid and reduced sugar occur slow non-enzymatic browning and generate a variety of aldoketones and the heterocyclic compound with roasting fragrance,
In certain amino acid such as phenylalanine be benzyl alcohol, benzyl carbinol precursor, itself can resolve into fragrance under suitable condition
Compound.
Small-micelle water of the present invention can be improved the permeability of amino acid, and the content for penetrating into it in tobacco increases,
Strength and richness are inhaled to improve the product of tobacco, a certain amount of amino acid is dissolved with small-micelle water of the present invention, is configured to spy
The amino acid solution for determining concentration is sprayed at tobacco surface, the tobacco dried wash with distilled water, pours into 0.03M hydrochloric acid solution and surpasses
Sonication 60min detects the content of amino acid with liquid chromatogram-high-resolution tandem mass spectrometer (miorOTOF-QII) after filtering,
Table 2 indicates four kinds of different water samples: Yunnan Zhong Yan company water sample (A), certain commercially available brand water sample (B), the embodiment of the present invention 1 are made
Water sample (C), control blank water sample (distilled water) (D) detect ammonia after preparing the amino acid solution sprinkling tobacco leaf of same concentrations respectively
The content of base acid.The results are shown in Table 2.
Table 2: amino acid content after different water sample processing tobaccos
As shown in Table 2, its interior amino acid content reaches after water sample (C) processing tobacco leaf is made in the embodiment of the present invention 1
748.08 μm of ol/L are significantly improved compared with the control blank water sample (distilled water) (D) for not spraying amino acid solution, and high
Its interior amino acid content after certain commercially available brand water sample (B) handles tobacco leaf.This experiment shows small-micelle water of the invention to ammonia
The permeability of base acid improves a lot, and is good solvent in tobacco processing, and the mouthfeel for being conducive to tobacco finished product is promoted.
The above content is the further descriptions for combining specific preferred embodiment to make the present invention.For this
For the those of ordinary skill of technical field that the present invention belongs to, the obvious variant made without departing from the inventive concept of the premise,
Performance or purposes are identical, are regarded as protection scope of the present invention.
Claims (2)
1. a kind of preparation method of small-micelle water, which is characterized in that method includes the following steps:
(1) pure water at room temperature is cooled down with the rate of 0.5 DEG C/min, when reaching each critical point, keeps temperature
30~60min then proceedes to cool down；When reaching 0 DEG C, 30~60min of temperature is kept；Then again with 0.2 DEG C/min rate drop
Temperature keeps 30~60min of temperature when reaching each critical point；Continue to cool down, when temperature reaches -6 DEG C, keeps temperature 30
~60min, obtains solid ice；
(2) solid ice for obtaining step (1), is heated up with the rate of 0.2 DEG C/min, and the heating-up time is 120~210min
Afterwards, then with 0.5 DEG C/min rate it heats up, reaches after room temperature to get to the small-micelle water；The subset
Water17O-NMR half-peak breadth numerical value is 48.6Hz, and hydrogen-free stroke degree is 34.18%；
The critical point is 10 DEG C, 5 DEG C, 2 DEG C, 0 DEG C, -2 DEG C, -5 DEG C, -6 DEG C；The room temperature is 20~25 DEG C.
2. small-micelle water prepared by preparation method according to claim 1 is for improving infiltration of the amino acid to tobacco
The purposes of rate.
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| CN201610316880.2A CN105800719B (en) | 2016-05-12 | 2016-05-12 | The preparation method and its purposes in tobacco of a kind of small-micelle water |
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| CN112834549A (en) * | 2021-02-05 | 2021-05-25 | 河北中烟工业有限责任公司 | Method for screening and evaluating small molecule cluster water in tobacco processing process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102415611A (en) * | 2011-07-24 | 2012-04-18 | 红云红河烟草(集团)有限责任公司 | Tobacco charging method for improving using effect of tobacco flavor |
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| JPS5396250A (en) * | 1977-02-02 | 1978-08-23 | Takasago Thermal Eng Co Lts | Heat accumulated water tank for purifying gushed-out contaminated heat accumulated water |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102415611A (en) * | 2011-07-24 | 2012-04-18 | 红云红河烟草(集团)有限责任公司 | Tobacco charging method for improving using effect of tobacco flavor |
Non-Patent Citations (1)
| Title |
|---|
| 不同尺度水分子簇生物效应的研究;师留印;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20111215(第S2期);中文摘要，正文第19-27页第2.1-2.5节 * |
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