CN105800719A - Preparation method of subset water and use of subset water in tobaccos - Google Patents
Preparation method of subset water and use of subset water in tobaccos Download PDFInfo
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- CN105800719A CN105800719A CN201610316880.2A CN201610316880A CN105800719A CN 105800719 A CN105800719 A CN 105800719A CN 201610316880 A CN201610316880 A CN 201610316880A CN 105800719 A CN105800719 A CN 105800719A
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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
-
- 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)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Indole Compounds (AREA)
Abstract
The invention discloses a preparation method of subset water. The preparation method comprises the following steps: (1) cooling purified water at the room temperature in a velocity of 0.5 DEG C/min, maintaining the temperature for 30-60 minutes at each critical point, further cooling, maintaining the temperature for 30-60 minutes when the temperature is 0 DEG C, cooling in a velocity of 0.2 DEG C/min, maintaining the temperature for 30-60 minutes at each critical point, further cooling, and maintaining the temperature for 30-60 minutes when the temperature is -6 DEG C, so as to obtain solid ice; and (2) heating the solid ice obtained in the step (1) for 120-210 min at a velocity of 0.2 DEG C/min, and then heating at a velocity of 0.5 DEG C/min until reaching the room temperature, so as to obtain subset water.
Description
Technical field
The present invention relates to a kind of purified water and preparation method and purposes, particularly to the preparation method of small-micelle water
And the purposes in Nicotiana tabacum L..
Background technology
Water, as the necessary of life, along with the day by day raising of people's living standard, has been sent to higher
Expect and requirement.Water in nature is presented in molecular structure.Hydrone under the effect of hydrogen bond,
Bigger micel can be formed, and bigger micel is unfavorable for the human body absorption to water.The micel of water is the least,
The penetration of water is the strongest, is more easy to enter cell membrane, transports nutriment, take the rubbish of cell out of.
Water is made up of two hydrogen atoms and an oxygen atom, and the two hydrogen atom is not former with oxygen in 180 degree
Sub-line connection, but be distributed in V-shape.The constitution element of water and molecular structure make it have many
Unique character, the particularly formation of hydrogen bond.Its structure has two receptors that can produce hydrogen bond and generation respectively
Hydrogen bond give body, produced different water-bounds between hydrone by the formation of hydrogen bond, as being similar to the four sides of ice
Body, dimer and polymer.
Hydrogen bond is a kind of slightly stronger than intermolecular force (Van der Waals force), more weak than covalent bond and ionic bond a lot
Interacting, its stability is weaker than covalent bond and ionic bond.In aqueous water, by stronger between several hydrones
Hydrogen bond action combines, and molecular association i.e. occurs, and forms (H2O) molecular cluster of n.Hydrogen between hydrone
Key average bond energy is 21kJ/mol, when temperature, pressure change or by External Force Acting, it is provided that extra energy breaks
Hydrogen bond between bad hydrone, and the chemical bond in hydrone is not destroyed, the available less little molecule of cluster number
Group's water.Hydrogen bond dissociation energy is 110kJ/mol, and its strong energy is neither big nor small, it is easy to connects and is also easy to fracture.
So among the Cluster Structures of water clusters is always at constantly changing.
Research proves, passes through external energy, it is achieved the change of water molecule cluster number, such as magnetic field facture,
Electric field treatment method, microwave treatment method, tourmaline facture, these methods produce small-micelle water, and it is prepared
Small-micelle water poor stability, returns to again macromolecular mass tufted state after long-time placement, and these methods can not
Seriality operates, production efficiency is low, less economical, and preparation is time-consuming long.
Summary of the invention
Present invention aims to existing technical scheme exist poor stability, can not seriality operation,
The problem such as less economical, it is provided that a kind of new small-micelle water preparation method.
First aspect present invention relates to the preparation method of a kind of small-micelle water, and the method comprises the following steps:
(1) pure water at room temperature is lowered the temperature with the speed of 0.5 DEG C/min, when reaching each critical point,
Keep temperature 30～60min, then proceed to cooling；When reaching 0 DEG C, keeping temperature 30～60min；So
After again with 0.2 DEG C/min speed lower the temperature, when reaching each critical point, keep temperature 30～60min；Continue
Cooling, when temperature reaches-6 DEG C, keeps temperature 30～60min, obtains solid ice；
(2) solid ice step (1) obtained, heats up with the speed of 0.2 DEG C/min, the heating-up time
After being 120～210min, then heat up with 0.5 DEG C/min speed, after reaching room temperature, i.e. obtain described
Small-micelle water.
Preferably, described critical point is 10 DEG C, 5 DEG C, 2 DEG C, 0 DEG C ,-2 DEG C ,-5 DEG C ,-6 DEG C；Described room
Temperature is 20～25 DEG C.
Second aspect present invention relate to small-micelle water prepared by the preparation method of described small-micelle water for
Improve the purposes of the aminoacid permeability to Nicotiana tabacum L..
Beneficial effects of the present invention:
1, the preparation method is that by energy exchange produced by ice-out Cheng Shui after freezing, make moisture
The kinetic energy of sub-cluster increases, and the amplitude in equilbrium position increases the most therewith, thus chemical bond goes out in Cluster Structures
Existing a certain degree of bending, changing of the O-H key angular separation of certain molecule of centrage and its of adjacent hydrone
Become, it will cause the fracture of hydrogen bond, effectively preparation method is simplified, directly change the structure of water molecule cluster,
Having can the advantage such as seriality operation, formation efficiency height, good economy performance.
2, the preparation method of the present invention realizes the macromole cluster of water is refined into subset bunch, water sample17O
NMR half-peak breadth numerical value is low, and Raman spectrum hydrogen-free linkage content is high, good stability, and solvability is high, can be more preferably
Ground is in agricultural, industrial aspect application.
3, amino acid whose permeability is improved a lot by small-micelle water of the present invention, is fine in Nicotiana tabacum L. processing
Solvent, in Nicotiana tabacum L., beneficially Nicotiana tabacum L. finished product mouthfeel promote.
Accompanying drawing explanation
Fig. 1 is the specific embodiment schematic diagram of the inventive method.
Fig. 2 is the inventive method and other water samples17O liquid core magnetic value；Wherein A is Yunnan Zhong Yan company
Water sample, B be certain company's water sample, C be certain brand water sample commercially available, D be the embodiment of the present invention 1 prepare water sample,
E is distillation water sample (blank water sample).
Fig. 3 is that the subset water sample that the inventive method prepares prepares water sample with additive method17O liquid core
Magnetic value；1 be tourmaline method process water sample, 2 be Magnitizing method process water samples, 3 be at electrolytic method
The water sample of reason, 4 be the embodiment of the present invention 1 prepare water sample, 5 be distillation water sample (blank water sample).
Fig. 4 is succi Nicotiana tabacum L. sample in Yunnan, certain brand water sample commercially available, the subset water sample of the present invention and distilled water
The Raman swarming spectrogram of sample (blank water sample)；
Detailed description of the invention
As it is shown in figure 1, be a kind of device utilizing Refrigeration Technique to prepare small-micelle water, this device includes glass
Container 1, glass container interlayer 5, water inlet pipe 3, outlet pipe 4, refrigeration system 2, in described refrigeration system 2
Including control chamber, circulating pump, refrigeration plant, refrigeration system 2 and water inlet pipe 3, glass container interlayer 5, go out
Water pipe 4 connects into a circulating device；Described glass container 1 is a system closed, and is artificial foundation
Second constant temperature field, loads former water source in glass container 1；Cold-producing medium in refrigeration system 2 is through water inlet pipe 3
Flow into glass container interlayer 5 to outflow back in refrigeration system 2 from outlet pipe 4.
The inventive method provide the Raman spectrum preparing small-micelle water,17The spies such as O-NMR liquid core magnetic value
Property, wherein17What 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 aqueous water self particularity, its17O-NMR spectral line spectral line width in all Isotopes spectral lines is the narrowest, therefore is utilizing nuclear magnetic resonance, NMR to aqueous water
Should select when studying17O core measures.Due to transverse relaxation process spin states between core
Exchange, and the Cluster Structures of water is the biggest, between oxygen core and neighbouring core, the exchange of spin states is the fastest, and sample is extensive
The shortest to the time required for equilibrium state again, spectral line is the widest, therefore, utilizes the width of Nmr Lines
Can be with the average relative size of reflecting liquid water cluster structure, spectral line is the widest, and cluster is the biggest；Spectral line is the narrowest, group
Bunch the least.17O-NMR half-peak breadth can be used for representing the characteristic of the small-micelle water of the present invention.
Raman spectrum is usually used in studying the performance of hydrone active force, Raman shift about 2600-4000cm-1Representative
The OH stretching vibration for hydrone, Gaussian function swarming the signal of this scope can be separated five bands
(band), principle during different water sample swarming is, the positions of five bands are the most fixing, use each water sample
Half-breadth high level all as, its center position respectively be about 3018, about 3223, about 3393, about 3506 and
About 3624cm-1, first three position contributed by the strong hydrogen bonding between hydrone, and rear both main are respectively weak hydrogen bonds
And the composition without hydrogen bond, the integral area of both bands rear is divided by the value of the area summation of five bands, the amount of being defined as
The percentage composition of degree without hydrogen bond (without hydrogen bond force strength) representative in the hydrone surveyed.General and
Speech, the degree without hydrogen bond of deionized water is 21.29%.When hydrogen bond is destroyed, show in Raman spectrum,
The band strength (area) of strong hydrogen bonding reduces, and is instead that weak hydrogen bond rises with the band strength without hydrogen bond, because of
This, Raman spectrum can be used for representing the characteristic of the small-micelle water of the present invention.
Following instance is the further labor to the present invention, but embodiments of the present invention are not limited to this.
Embodiment 1: the preparation of small-micelle water of the present invention
By in water sample load map 1 glass container 1 of Yunnan Zhong Yan company, cold-producing medium loads refrigeration system 2, adjusts
The temperature program of joint control chamber refrigeration plant, the temperature program of control chamber regulation refrigeration plant, control tank cooling
Speed is 0.5 DEG C/min, when cooling to each critical point (10 DEG C, 5 DEG C, 2 DEG C, 0 DEG C), controls temperature
Stablize 30-60min, continue cooling afterwards, be cooled to occur during trash ice (when 0 DEG C), then control rate of temperature fall
It is 0.2 DEG C/min, continues to be cooled to critical point (-2 DEG C ,-5 DEG C ,-6 DEG C), control temperature stabilization 30-60min,
When liquid becomes solid in glass container, stop cooling, when the freezing of former water source is solid, then control tank
Heating rate is 0.2 DEG C/min, heats up after 120～210min, then to regulate heating rate be 0.5 DEG C/min liter
To room temperature, in glass container, obtain the small-micelle water with subset bunch characteristic.
Embodiment 2: the liquid nuclear-magnetism of small-micelle water of the present invention and other water samples
Yunnan Zhong Yan company water sample (A), certain company's water sample (B), certain brand water sample (C) commercially available, reality
Execute that example 1 prepares water sample (D), blank water sample (E) is carried out17O magnetic resonance detection, A, B, C,
D, E water sample is respectively charged in nuclear magnetic tube, with Liquid NMR instrument (Liquid Nuclear Magnetic
Resonance, model AVANCE III, purchased from Brooker) detect, nuclear magnetic tube is put into nuclear-magnetism altogether
In Vibration Meter, scan 516 times, obtained the width of Nmr Lines by the free quantum signal of O core, enter
And half-value width can be obtained.
According to nuclear-magnetism result it is known that embodiment 1 the most successfully prepares small-micelle water.Yunnan Zhong Yan company
Water sample (A) nuclear-magnetism value is 68.1Hz, and it is 48.6Hz that embodiment 1 prepares water sample (D), half-value width
There is significantly reduction, subset bunch less (with reference to accompanying drawing 2) is described.
Embodiment 3: small-micelle water prepared by the inventive method and other inventive methods prepare watery liquid core
Magnetic value compares
Water sample (2), electrolytic method that the water sample (1) of tourmaline method process, Magnitizing method are processed process
Water sample (3), the water sample (4) for preparing of embodiment 1 and blank water sample (5) of organizing carry out17O nuclear magnetic resonance, NMR
Detection, is respectively charged into 1,2,3,4,5 water samples in nuclear magnetic tube, with Liquid NMR instrument (Liquid Nuclear
Magnetic Resonance, model AVANCE III, purchased from Brooker) detect, nuclear magnetic tube is put
Enter in nuclear magnetic resonance analyser, scan 516 times, obtain Nmr Lines by the free quantum signal of O core
Width, and then half-value width can be obtained.
According to nuclear-magnetism result it is known that its half-value width of water sample minimum (48.6 of preparing of the embodiment of the present invention 1
Hz), namely the method for embodiment 1 can obtain the less water of molecular cluster (with reference to the post 4 of accompanying drawing 3).
Embodiment 4: small-micelle water of the present invention and the Raman spectrum of other water samples
Yunnan Zhong Yan company water sample (A), certain brand water sample (B) commercially available, the embodiment of the present invention 1 are prepared
Subset water sample (C), blank water sample (distilled water) (D) carry out Raman spectrum analysis, water sample
Drop on microscope slide, be wherein coated with the square silver strip of 0.1mm thickness on microscope slide, with laser Raman spectroscopy
Instrument (Laser Raman Spectrometer, model inVia reflex, purchased from thunder Manny) detects, carrying
The microscope slide having water sample is put under the microscope, with the laser of wavelength 532 nanometer at measuring range 2800-3800
cm-1In, each time of exposure is 30 seconds, after scanning 1 time, obtains OH stretching vibration signal and goes forward side by side line number
According to swarming analysis.Different water sample Raman spectrum swarming figures are shown in Fig. 4.
OH stretching vibration signal swarming position is set in 3018cm by spectroscopic data swarming analysis-1、3223
cm-1、3393cm-1、3506cm-1, and 3624cm-1, and during each sample swarming, use each water sample
Band half-breadth high level all as.Wherein it is positioned at 3506cm-1And 3624cm-1It is belonging respectively to weak hydrogen bond and without hydrogen bond
The area of composition band, with the area ratio of overall OH stretching vibration band, be defined as without hydrogen bond degree.Raman
Results of spectral measurements, as shown in table 1.
Table 1: the Raman light spectrum of different water samples
Understanding from form, the degree without hydrogen bond that the embodiment of the present invention 1 prepares water sample (C) is the highest, reaches
34.18%, the 12.53% of the blank water sample (distilled water) of comparison, obvious the inventive method has successfully been prepared little
Micel water.
Embodiment 5: small-micelle water osmotic effect of the present invention
Aminoacid is that the class important substance in Nicotiana tabacum L. has significant contribution in terms of tobacco incense flavor quality, is synthesis egg
White matter and the raw material of nicotine, aminoacid appropriate in Nicotiana tabacum L. is favorably improved flue gas strength and increases richness.One
Aspect, aminoacid burning can produce the nitrogen-containing compound such as NH affecting flue gas mass3；On the other hand, flue-cured tobacco exists
Modulation, refine and ferment during, there is the multiple aldehyde of non-enzymatic browning generation slowly in free amino acid and reducing sugar
Ketone and have the heterocyclic compound of roasting fragrance, some of which aminoacid such as phenylalanine is benzyl alcohol, benzene second
The precursor of alcohol, but self resolves into perfume compound under suitable condition.
Small-micelle water of the present invention can improve amino acid whose permeability so that it is penetrates into the content in Nicotiana tabacum L. and increases
Many, thus the product improving Nicotiana tabacum L. inhale strength and richness, with a certain amount of amino of subset water dissolution of the present invention
Acid, the Freamine Ⅲ being configured to certain concentration is sprayed at Nicotiana tabacum L. surface, cleans the Nicotiana tabacum L. dried with distilled water,
Pour supersound process 60min in 0.03M hydrochloric acid solution into, with liquid chromatograph-high-resolution tandem mass spectrometer after filtration
(miorOTOF-QII) detecting amino acid whose content, table 2 represents four kinds of different water samples: in Yunnan, cigarette is public
Sample (A), certain brand water sample (B) commercially available, the embodiment of the present invention 1 of water tendering prepares water sample (C), comparison sky
Plain boiled water sample (distilled water) (D), the Freamine Ⅲ preparing same concentrations respectively sprays detection amino after Nicotiana tabacum L.
The content of acid.Result is as shown in table 2.
Table 2: different water samples process amino acid content after Nicotiana tabacum L.
As shown in Table 2, the embodiment of the present invention 1 prepares amino acid content in water sample (C) processes after Nicotiana tabacum L. it and reaches
To 748.08 μm ol/L, with do not spray Freamine Ⅲ compare blank water sample (distilled water) (D) phase
Ratio is significantly improved, and processes after Nicotiana tabacum L. amino acid content in it higher than certain brand water sample (B) commercially available.This
Experiment shows, amino acid whose permeability is improved a lot by the small-micelle water of the present invention, is in Nicotiana tabacum L. processing
Well the mouthfeel of solvent, beneficially Nicotiana tabacum L. finished product promotes.
Above content is to combine the further description that the present invention is made by concrete preferred implementation.Right
For general technical staff of the technical field of the invention, make without departing from the inventive concept of the premise
Obvious modification, performance or purposes are identical, are regarded as protection scope of the present invention.
Claims (3)
1. the preparation method of a small-micelle water, it is characterised in that the method comprises the following steps:
(1) pure water at room temperature is lowered the temperature with the speed of 0.5 DEG C/min, when reaching each critical point,
Keep temperature 30～60min, then proceed to cooling；When reaching 0 DEG C, keep temperature 30～60min；Then
Lower the temperature with 0.2 DEG C/min speed again, when reaching each critical point, keep temperature 30～60min；Continue fall
Temperature, when temperature reaches-6 DEG C, keeps temperature 30～60min, obtains solid ice；
(2) solid ice step (1) obtained, heats up with the speed of 0.2 DEG C/min, the heating-up time
After being 120～210min, then heat up with 0.5 DEG C/min speed, after reaching room temperature, i.e. obtain described
Small-micelle water.
Preparation method the most according to claim 1, it is characterised in that described critical point is 10 DEG C, 5 DEG C,
2℃、0℃、-2℃、-5℃、-6℃；Described room temperature is 20～25 DEG C.
Small-micelle water prepared by preparation method the most according to claim 1 be used for improving aminoacid to
The purposes of the permeability of Nicotiana tabacum L..
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| CN105800719A true CN105800719A (en) | 2016-07-27 |
| CN105800719B CN105800719B (en) | 2018-12-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
-
2016
- 2016-05-12 CN CN201610316880.2A patent/CN105800719B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
|---|
| 师留印: "不同尺度水分子簇生物效应的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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