CN107880856A - A kind of paraffin wax emulsions ice slurry and preparation method thereof - Google Patents
A kind of paraffin wax emulsions ice slurry and preparation method thereof Download PDFInfo
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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Abstract
The invention discloses a kind of paraffin wax emulsions ice slurry and preparation method thereof, belong to cool storage material preparing technical field.The present invention uses atoleine, emulsifying agent, anti-adhesion agent, hollow Nano pearl, organosilicon and water as raw material, first organosilicon, emulsifying agent, anti-adhesion agent and water are poured into glass beaker, after high-speed stirred mixing, add atoleine, emulsifying, obtain emulsion, to fill again the glass beaker of emulsion in temperature be in 0.8~0.4 DEG C of air bath, and add hollow Nano pearl, 2~4h of stirring reaction, discharging, produces paraffin wax emulsions ice slurry, wherein, hollow Nano pearl is to react to obtain by ferrous nitrate, ferric nitrate, water and ammoniacal liquor.Gained paraffin wax emulsions ice slurry ice-storage rate of the invention is effectively improved, and solves the problems, such as that the low ice that easily occurs of ice-storage rate blocks up.
Description
Technical field
The invention discloses a kind of paraffin wax emulsions ice slurry and preparation method thereof, belong to cool storage material preparing technical field.
Background technology
Ice slurry is the solid-liquid two phase liquid of suspension ice crystalses and water, has big storage density of cold, good fluidity, transports conveniently
The features such as, it is excellent agent for storage of coldness and refrigerating medium.Because ice slurry has good flowing and heat transfer property, storage is widely used in
The fields such as cold, air-conditioning, food processing preservation and mine cooling, " peak load shifting " of electric power can be effectively realized, it is wide by scholars
General concern.
Ice slurry is a kind of mixture of ice and water, also known as fluidic ice, binary ice, pumpable ice.There is scholar by the substantially special of ice slurry
Sign is defined as by aqueous water and with average characteristic diameter no more than the paste mixture that 1mm ice crystalses form.From 20th century
The nineties, food products market increasingly required that fresh food replaces frozen food till now.Current manual can produce different
Ice（Trash ice, ice bits, ice slurry etc.）, they play different effects in food fresh keeping cooling.Ice crystal size in ice slurry compared with
It is small, profile rule so that ice slurry is soft, can be by food（Such as fish, meat and fruits and vegetables）It is immersed in ice slurry without damaging
Get ill from overeating the tissue and appearance of product, and because ice slurry completely can submerge food, completely cut off contact of the food with air, can press down
The breeding of bacterium processed, it is effectively protected the quality of food.And because ice slurry has good mobility, flexible pipe can be passed through
Or common Pipeline transport, the terminal of such equipment can be placed arbitrarily, easy to use laborsaving.A variety of factors show that ice slurry is being eaten
There is preferable development prospect in product freezing and refrigeration.
Effective preparation of ice slurry is that the premise that ice slurry is applied as agent for storage of coldness and refrigerating medium and basis, its preparation method are main
Including Supercool method, mechanical facing, fluidized bed process, vacuum method, contact method etc..Supercool method, fluidized bed process and directly contact
Method has the advantages of heat exchange efficiency is high, but the problem of blocked up there is also Yi Bing；Facing ice making efficiency high, problem is blocked up without ice, but be
System is complicated, needs periodic replacement scraper, efficiency low；And vacuum rule requires higher to vacuum and air-tightness, system is huge.Always
For body, subcooled water preparation ice slurry has the advantages that simple system, initial cost are low, heat exchange efficiency is high, in widespread attention.
In ice slurry producing process, ice slurry effectively produce, ice content control with adhesion wall prevent be ice slurry prepare
The key factor of process.The effective ways that appropriate alcohol and inorganic salts are preparing ice slurries are added in water.Paraffin breast traditional at present
There is the problem of ice-storage rate is low, and easily generation ice is stifled in liquid ice slurry, inquire into ice slurry and prepare new way, it is very heavy to simplify ice slurry preparation system
Will.
The content of the invention
The present invention solves the technical problem of：It is low for prior paraffin emulsion ice slurry ice-storage rate, ice easily occurs and blocks up, carries
A kind of paraffin wax emulsions ice slurry and preparation method thereof is supplied.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of paraffin wax emulsions ice slurry, it is characterised in that：Include the raw material of following parts by weight：
10~15 parts of atoleine
3~5 parts of emulsifying agent
8~10 parts of anti-adhesion agent
8~10 parts of hollow Nano pearl
4~8 parts of organosilicon
100~120 parts of water
The specific preparation process of hollow Nano pearl is：Count in parts by weight, take 18~20 parts of ferrous nitrates successively, 45~50 parts
Ferric nitrate, 200~300 parts of water, is stirred dissolving, obtains mixed solution, then molten to mixed solution and dripping ammoniacal liquor, regulation mixing
Liquid pH to 8.0~8.2, add 0.01~0.03 times of the gellan gum and mixed solution quality of 0.1~0.2 times of mixed solution quality
Tween-60, after being stirred, be incubated still aging 2~4h, then after being concentrated under reduced pressure, low temperature spray drying, obtain hollow Nano
Pearl；
The specific preparation process of paraffin wax emulsions ice slurry is：
（1）Formed by raw material and weigh each component；
（2）Organosilicon, emulsifying agent, anti-adhesion agent and water are poured into glass beaker, after high-speed stirred mixing, add liquid stone
Wax, emulsifying, obtain emulsion；
（3）Hollow Nano pearl is added into the glass beaker for fill emulsion, then will fill the glass beaker of emulsion in temperature for-
In 0.8~-0.4 DEG C of air bath, 2~4h of stirring reaction, discharging, paraffin wax emulsions ice slurry is produced.
The emulsifying agent is formed by the raw material compounding of following parts by weight：20~30 parts of soybean lecithins, 10~15 parts
Neopelex, 20~30 parts of Tea Saponins.
The anti-adhesion agent is any one in absolute methanol, absolute ether or absolute ethyl alcohol.
The organosilicon is any one in methyl trifluoro propyl silicone oil, methyl phenyl silicone oil or MethylethoxylsiliconFluid Fluid
Kind.
The condition of being concentrated under reduced pressure is：Temperature is 75~80 DEG C, and pressure is 400~500kPa, and concentration time is 6~8h.
The low temperature spray drying condition is：Feed rate is 25~35g/min, and EAT is 95~100 DEG C, air-out
Temperature is 75~80 DEG C.
The beneficial effects of the invention are as follows：
（1）Technical solution of the present invention is added into system and is prepared by materials such as ferrous nitrate, ferric nitrate, ammoniacal liquor and gellan gums
Hollow Nano pearl, during hollow Nano pearl is prepared, ferrous nitrate and ferric nitrate can be under the alkaline systems that ammoniacal liquor provides
It is transformed into the magnetic nano ferriferrous oxide of tool, in ageing process, caused nano ferriferrous oxide is adsorbable and disperses
In gellan gum gelling system, it is added in paraffin wax emulsions ice slurry preparation process, hollow Nano pearl can induce and promote moisture fast
Speed, which freezes, forms ice crystal, and gellan gum contained therein is met water-swellable, can effectively keep the outstanding of the hollow heart nano-beads of system and ice crystal
Floating stability, and the holding of hollow Nano pearl suspension stability, can make each corner of system is dispersed to have hollow nano-beads, so as to
Be advantageous to induce and promote each corner of system quickly to form ice crystal, and well suspended avoids system layering in system, improves and stores
Ice rate；
（2）Technical solution of the present invention during paraffin wax emulsions ice slurry is prepared, considered critical use glass material beaker, and
Organosilicon is added in product preparation process, because organosilicon can be effectively formed hydrophobic membrane on glass container surface, and is added in emulsifying agent
The soybean lecithin added is also parental type molecule, and the hydrophobic membrane that its oleophylic side can be formed with organosilicon is well compatible, and hydrophilic
Side can system it is well compatible, so as on container wall formed organosilicon-phospholipid bilayer lubrication system, effectively avoid ice crystal from coagulating
Tie on container wall, effectively solved so that ice blocks up problem.
Embodiment
Count in parts by weight, take 18~20 parts of ferrous nitrates successively, 45~50 parts of ferric nitrates, 200~300 parts of water, pour into
In beaker, 20~30min of dissolving is stirred with glass bar, obtains mixed solution, then the beaker for filling mixed solution is moved into number
The aobvious constant temperature blender with magnetic force that tests the speed, it is 45~55 DEG C in temperature, under the conditions of speed of agitator is 300~500r/min, passes through dropping liquid
Mass fraction is added dropwise as 15~20% ammoniacal liquor into beaker using 3~5mL/min speed in funnel, adjust beaker in mixed solution pH to
8.0~8.2, add the gellan gum of 0.1~0.2 times of mixed solution quality and telling for 0.01~0.03 times of mixed solution quality
Temperature -60, continue constant temperature and be stirred 45~60min, stop stirring, be incubated still aging 2~4h, obtain ageing liquid, and by gained
It is aged liquid and moves into Rotary Evaporators, is 75~80 DEG C in temperature, under the conditions of pressure is 400~500kPa, be concentrated under reduced pressure 6~8h,
Concentrate, and gained concentrate is delivered to spray dryer with 25~35g/min feed rates, in EAT be 95~
100 DEG C, under the conditions of leaving air temp is 75~80 DEG C, cold nebulization is granulated, and obtains hollow nano-beads；Count, take successively in parts by weight
10~15 parts of atoleines, 3~5 parts of emulsifying agents, 8~10 parts of anti-adhesion agents, 8~10 parts of hollow Nano pearls, 4~8 parts of organosilicons,
100~120 parts of water, first pour into organosilicon, emulsifying agent, anti-adhesion agent and water in glass beaker, with agitator with 1600~
After 1800r/min rotating speeds high-speed stirred mixes 45~60min, then atoleine is added into glass beaker, and by glass beaker
Homogeneous emulsifying machine is moved into, under the conditions of temperature is 25~30 DEG C, 30~45min is emulsified, obtains emulsion；Then to the glass for filling emulsion
Hollow Nano pearl is added in glass beaker, then the glass beaker for filling emulsion is moved into -0.8~-0.4 DEG C of air bath, insulation
After 2~4h of stirring reaction, discharging, paraffin wax emulsions ice slurry is produced.The emulsifying agent be by following parts by weight raw material compounding and
Into：20~30 parts of soybean lecithins, 10~15 parts of neopelexes, 20~30 parts of Tea Saponins.The anti-adhesion agent is nothing
Any one in water methanol, absolute ether or absolute ethyl alcohol.The organosilicon is methyl trifluoro propyl silicone oil, aminomethyl phenyl silicon
Oil or MethylethoxylsiliconFluid Fluid in any one.
Example 1
Count in parts by weight, take 20 parts of ferrous nitrates successively, 50 parts of ferric nitrates, 300 parts of water, pour into beaker, stirred with glass bar
Mixed dissolution 30min is mixed, obtains mixed solution, then the beaker for filling mixed solution immigration digital display is tested the speed constant temperature blender with magnetic force,
It is 55 DEG C in temperature, under the conditions of speed of agitator is 500r/min, matter is added dropwise into beaker with 5mL/min speed by dropping funel
Amount fraction is 20% ammoniacal liquor, adjusts mixed solution pH to 8.2 in beaker, adds the gellan gum of 0.2 times of mixed solution quality and mixes
The Tween-60 of 0.03 times of solution quality is closed, continues constant temperature and is stirred 60min, stop stirring, be incubated still aging 4h, obtain old
To change liquid, and gained ageing liquid is moved into Rotary Evaporators, be 80 DEG C in temperature, under the conditions of pressure is 500kPa, be concentrated under reduced pressure 8h,
Concentrate is obtained, and gained concentrate is delivered to spray dryer with 35g/min feed rates, is 100 DEG C in EAT, goes out
Under the conditions of air temperature is 80 DEG C, cold nebulization is granulated, and obtains hollow nano-beads；Count in parts by weight, take 15 parts of atoleines successively,
5 parts of emulsifying agents, 10 parts of anti-adhesion agents, 10 parts of hollow Nano pearls, 8 parts of organosilicons, 120 parts of water, first by organosilicon, emulsifying agent, anti-stick
Agent and water are poured into glass beaker, after mixing 60min with agitator with 1800r/min rotating speeds high-speed stirred, then to glass beaker
Middle addition atoleine, and glass beaker is moved into homogeneous emulsifying machine, under the conditions of temperature is 30 DEG C, 45min is emulsified, is obtained newborn
Liquid；Then to addition hollow Nano pearl in the glass beaker for filling emulsion, then -0.4 DEG C of the glass beaker immigration of emulsion will be filled
Air bath in, insulated and stirred reaction 4h after, discharging, produce paraffin wax emulsions ice slurry.The emulsifying agent is by following parts by weight
Raw material compounding form：30 parts of soybean lecithins, 15 parts of neopelexes, 30 parts of Tea Saponins.The anti-adhesion agent is nothing
Water methanol.The organosilicon is methyl trifluoro propyl silicone oil.
Example 2
Count in parts by weight, take 20 parts of ferrous nitrates successively, 50 parts of ferric nitrates, 300 parts of water, pour into beaker, stirred with glass bar
Mixed dissolution 30min is mixed, obtains mixed solution, then the beaker for filling mixed solution immigration digital display is tested the speed constant temperature blender with magnetic force,
It is 55 DEG C in temperature, under the conditions of speed of agitator is 500r/min, matter is added dropwise into beaker with 5mL/min speed by dropping funel
Amount fraction is 20% ammoniacal liquor, adjusts mixed solution pH to 8.2 in beaker, adds the gellan gum of 0.2 times of mixed solution quality and mixes
The Tween-60 of 0.03 times of solution quality is closed, continues constant temperature and is stirred 60min, stop stirring, be incubated still aging 4h, obtain old
To change liquid, and gained ageing liquid is moved into Rotary Evaporators, be 80 DEG C in temperature, under the conditions of pressure is 500kPa, be concentrated under reduced pressure 8h,
Concentrate is obtained, and gained concentrate is delivered to spray dryer with 35g/min feed rates, is 100 DEG C in EAT, goes out
Under the conditions of air temperature is 80 DEG C, cold nebulization is granulated, and obtains hollow nano-beads；Count in parts by weight, take 15 parts of atoleines successively,
5 parts of emulsifying agents, 10 parts of anti-adhesion agents, 10 parts of hollow Nano pearls, 120 parts of water, emulsifying agent, anti-adhesion agent and water are first poured into glass beaker
In, after mixing 60min with agitator with 1800r/min rotating speeds high-speed stirred, then atoleine is added into glass beaker, and will
Glass beaker moves into homogeneous emulsifying machine, under the conditions of temperature is 30 DEG C, emulsifies 45min, obtains emulsion；Then to the glass for filling emulsion
Hollow Nano pearl is added in glass beaker, then the glass beaker for filling emulsion is moved into -0.4 DEG C of air bath, insulated and stirred is anti-
After answering 4h, discharging, paraffin wax emulsions ice slurry is produced.The emulsifying agent is formed by the raw material compounding of following parts by weight：It is 30 parts big
Beans lecithin, 15 parts of neopelexes, 30 parts of Tea Saponins.The anti-adhesion agent is absolute methanol.
Example 3
Count in parts by weight, take 20 parts of ferrous nitrates successively, 50 parts of ferric nitrates, 300 parts of water, pour into beaker, stirred with glass bar
Mixed dissolution 30min is mixed, obtains mixed solution, then the beaker for filling mixed solution immigration digital display is tested the speed constant temperature blender with magnetic force,
It is 55 DEG C in temperature, under the conditions of speed of agitator is 500r/min, matter is added dropwise into beaker with 5mL/min speed by dropping funel
Amount fraction is 20% ammoniacal liquor, adjusts mixed solution pH to 8.2 in beaker, adds the gellan gum of 0.2 times of mixed solution quality and mixes
The Tween-60 of 0.03 times of solution quality is closed, continues constant temperature and is stirred 60min, stop stirring, be incubated still aging 4h, obtain old
To change liquid, and gained ageing liquid is moved into Rotary Evaporators, be 80 DEG C in temperature, under the conditions of pressure is 500kPa, be concentrated under reduced pressure 8h,
Concentrate is obtained, and gained concentrate is delivered to spray dryer with 35g/min feed rates, is 100 DEG C in EAT, goes out
Under the conditions of air temperature is 80 DEG C, cold nebulization is granulated, and obtains hollow nano-beads；Count in parts by weight, take 15 parts of atoleines successively,
5 parts of emulsifying agents, 10 parts of anti-adhesion agents, 10 parts of hollow Nano pearls, 8 parts of organosilicons, 120 parts of water, first by organosilicon, emulsifying agent, anti-stick
Agent and water are poured into glass beaker, after mixing 60min with agitator with 1800r/min rotating speeds high-speed stirred, then to glass beaker
Middle addition atoleine, and glass beaker is moved into homogeneous emulsifying machine, under the conditions of temperature is 30 DEG C, 45min is emulsified, is obtained newborn
Liquid；Then to addition hollow Nano pearl in the glass beaker for filling emulsion, then -0.4 DEG C of the glass beaker immigration of emulsion will be filled
Air bath in, insulated and stirred reaction 4h after, discharging, produce paraffin wax emulsions ice slurry.The emulsifying agent is by following parts by weight
Raw material compounding form：15 parts of neopelexes, 30 parts of Tea Saponins.The anti-adhesion agent is absolute methanol.It is described organic
Silicon is methyl trifluoro propyl silicone oil.
Example 4
Count in parts by weight, take 20 parts of ferrous nitrates successively, 50 parts of ferric nitrates, 300 parts of water, pour into beaker, stirred with glass bar
Mixed dissolution 30min is mixed, obtains mixed solution, then the beaker for filling mixed solution immigration digital display is tested the speed constant temperature blender with magnetic force,
It is 55 DEG C in temperature, under the conditions of speed of agitator is 500r/min, matter is added dropwise into beaker with 5mL/min speed by dropping funel
Amount fraction is 20% urea liquid, adjusts mixed solution pH to 8.2 in beaker, adds the gellan gum of 0.2 times of mixed solution quality
And the Tween-60 of 0.03 times of mixed solution quality, continue constant temperature and be stirred 60min, stop stirring, be incubated still aging 4h,
Liquid must be aged, and gained ageing liquid is moved into Rotary Evaporators, is 80 DEG C in temperature, under the conditions of pressure is 500kPa, decompression is dense
Contracting 8h, obtain concentrate, and gained concentrate be delivered to spray dryer with 35g/min feed rates, in EAT be 100
DEG C, under the conditions of leaving air temp is 80 DEG C, cold nebulization is granulated, and obtains hollow nano-beads；Count in parts by weight, take 15 parts of liquid successively
Paraffin, 5 parts of emulsifying agents, 10 parts of anti-adhesion agents, 10 parts of hollow Nano pearls, 8 parts of organosilicons, 120 parts of water, first by organosilicon, emulsifying agent,
Anti-adhesion agent and water are poured into glass beaker, after mixing 60min with agitator with 1800r/min rotating speeds high-speed stirred, then to glass
Atoleine is added in beaker, and glass beaker is moved into homogeneous emulsifying machine, under the conditions of temperature is 30 DEG C, 45min is emulsified, obtains
Emulsion；Then to addition hollow Nano pearl in the glass beaker for filling emulsion, then the glass beaker immigration -0.4 of emulsion will be filled
DEG C air bath in, insulated and stirred reaction 4h after, discharging, produce paraffin wax emulsions ice slurry.The emulsifying agent is by following parts by weight
Several raw material compoundings form：30 parts of soybean lecithins, 15 parts of neopelexes, 30 parts of Tea Saponins.The anti-adhesion agent is
Absolute methanol.The organosilicon is methyl trifluoro propyl silicone oil.
The gained paraffin wax emulsions of example 1 to 4 ice slurry is subjected to performance detection, detects its ice-storage rate, specific testing result such as table 1
It is shown：
Table 1
| Detection content | Example 1 | Example 2 | Example 3 | Example 4 |
| Ice-storage rate/% | 65 | 35 | 30 | 40 |
The gained paraffin wax emulsions ice slurry ice-storage rate of example 2,3,4 is low, and example 2 and the gained paraffin wax emulsions ice slurry of example 3 occur
The stifled phenomenon of ice.
From testing result, present invention gained paraffin wax emulsions ice slurry ice-storage rate is effectively improved, and solves ice-reserving
Rate is low easily to occur the problem of ice is stifled.
Claims (6)
- A kind of 1. paraffin wax emulsions ice slurry, it is characterised in that：Include the raw material of following parts by weight：10~15 parts of atoleine3~5 parts of emulsifying agent8~10 parts of anti-adhesion agent8~10 parts of hollow Nano pearl4~8 parts of organosilicon100~120 parts of waterThe specific preparation process of hollow Nano pearl is：Count in parts by weight, take 18~20 parts of ferrous nitrates successively, 45~50 parts Ferric nitrate, 200~300 parts of water, is stirred dissolving, obtains mixed solution, then molten to mixed solution and dripping ammoniacal liquor, regulation mixing Liquid pH to 8.0~8.2, add 0.01~0.03 times of the gellan gum and mixed solution quality of 0.1~0.2 times of mixed solution quality Tween-60, after being stirred, be incubated still aging 2~4h, then after being concentrated under reduced pressure, low temperature spray drying, obtain hollow Nano Pearl；The specific preparation process of paraffin wax emulsions ice slurry is：（1）Formed by raw material and weigh each component；（2）Organosilicon, emulsifying agent, anti-adhesion agent and water are poured into glass beaker, after high-speed stirred mixing, add liquid stone Wax, emulsifying, obtain emulsion；（3）Hollow Nano pearl is added into the glass beaker for fill emulsion, then will fill the glass beaker of emulsion in temperature for- In 0.8~-0.4 DEG C of air bath, 2~4h of stirring reaction, discharging, paraffin wax emulsions ice slurry is produced.
- A kind of 2. paraffin wax emulsions ice slurry according to claim 1, it is characterised in that：The emulsifying agent is by following parts by weight Several raw material compoundings form：20~30 parts of soybean lecithins, 10~15 parts of neopelexes, 20~30 parts of Tea Saponins.
- A kind of 3. paraffin wax emulsions ice slurry according to claim 1, it is characterised in that：The anti-adhesion agent is absolute methanol, nothing Any one in water ether or absolute ethyl alcohol.
- A kind of 4. paraffin wax emulsions ice slurry according to claim 1, it is characterised in that：The organosilicon is methyl trifluoro propyl Any one in silicone oil, methyl phenyl silicone oil or MethylethoxylsiliconFluid Fluid.
- A kind of 5. paraffin wax emulsions ice slurry according to claim 1, it is characterised in that：The condition of being concentrated under reduced pressure is：Temperature For 75~80 DEG C, pressure is 400~500kPa, and concentration time is 6~8h.
- A kind of 6. paraffin wax emulsions ice slurry according to claim 1, it is characterised in that：The low temperature spray drying condition is： Feed rate is 25~35g/min, and EAT is 95~100 DEG C, and leaving air temp is 75~80 DEG C.
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| CN109181599A (en) * | 2018-09-20 | 2019-01-11 | 薛向东 | A kind of composite modified alkyd resin adhesive |
| CN110256901A (en) * | 2019-06-12 | 2019-09-20 | 魏炎梅 | A kind of preparation method of cobalt blue ceramic glaze special-purpose ink |
| CN110317015A (en) * | 2019-06-12 | 2019-10-11 | 梁家杰 | A kind of composite high-strength concrete |
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| CN115197676A (en) * | 2022-06-23 | 2022-10-18 | 南京长江都市建筑设计股份有限公司 | Octanol system emulsion ice slurry and preparation method and application thereof |
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