CN109970929A - A kind of temperature sensitive type releases the preparation method of salt material - Google Patents
A kind of temperature sensitive type releases the preparation method of salt material Download PDFInfo
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- CN109970929A CN109970929A CN201910157715.0A CN201910157715A CN109970929A CN 109970929 A CN109970929 A CN 109970929A CN 201910157715 A CN201910157715 A CN 201910157715A CN 109970929 A CN109970929 A CN 109970929A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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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
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
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Abstract
The present invention relates to the preparation methods that a kind of temperature sensitive type releases salt material, belong to pavement construction material technical field.The present invention is using industrial alkali lignin as raw material, formaldehyde and N, N '-methylene-bisacrylamide is crosslinking agent, in the case where potassium peroxydisulfate/tetramethylethylenediamine redox system causes with acrylic acid, n-isopropyl acrylamide and acrylamide free yl graft polymerization, the temperature sensitive type for being prepared for a kind of three-dimensional network crosslinking releases salt material, industrial alkali lignin is aromatic polymer polymer made of being coupled as phenylpropyl alcohol alkyl structure unit by ehter bond and carbon-carbon bond, has stronger chelating ability and colloidal property；Persulfate slow-release material can generate the potentiometric titrations SO of strong oxidizing property under the conditions of transition metal-catalyzed4 ‑, and good oxidability is all had under acid, neutral, alkaline condition；The present invention can be rapidly frozen hydrogel sample by the way of liquid-nitrogen freeze drying, considerably reduce the surface tension effects in freezing and drying process hydrone.
Description
Technical field
The present invention relates to the preparation methods that a kind of temperature sensitive type releases salt material, belong to pavement construction material technical field.
Background technique
Since the weather of winter cold causes the frequent accumulated snow in road surface to freeze, and thus cause coefficient of road adhesion decline, vapour
The problems such as vehicle skidding, direction out of control, leads to serious traffic problems, bring very big influence to the coast is clear and traffic safety, because
This ensures road traffic safety and operational efficiency and passage energy unimpeded, and that improve road entirety to reduce traffic accident rate
Power, it is necessary to be purged using various measures and means road pavement ice and snow.Problem is avenged for road surface deicing, various countries are always very
Pay attention to, and made numerous studies, explores various roads deicing method, can be divided mainly into passive type and active two major classes.
Passive type snow-removing method refers to the method for removing ice and snow on road surfaces by extraneous road pavement, application effect, can be divided into physics, change
It learns, mechanical three classes.Active snow-removing method is using special tectonic characteristic possessed by road surface itself or mechanical characteristic, without outer
The booster action on boundary can actively remove the technology of road snow and solidifying ice under the repeated action of normal traffic load.
In recent years, active deicing technology increasingly obtains various countries' traffic and the attention of scientific research department, new active deicing
Snow technology also constantly emerges, wherein stores salt pavement technique as a kind of novel environmentally friendly active deicing
Technology has caused the concern of domestic and international traffic study person.Salt pavement technique is stored to refer to through different processing technologys to ice
Point depressant is handled, and is molded into the particle or powder of different-grain diameter, the mineral aggregate of different-grain diameter in replacing asphalt mixture,
The snow melt agent material that bituminous pavement has active deicing traditional does not have slow-release function, is added in pavement material, after rainy season just
It is released and finishes, lose snow melting function to winter.
Realize that pavement material releases the project that the control always pavement construction material field of salt rate is related to, common method
It is to coat organic slow-release material for controlling rate of dissolution on dissolvable salt surface.Or salt dissolution is loaded into porous
Then material is modified with hydrophobic organic material, by multiple steps, finally obtain and release salt material with certain sustained release performance
Material.
Existing road with release salt material no matter Europe V260, or Japan's MFL product do not have temperature-sensing property, is used for
In pavement material, rainwater season in summer is lost serious.
Intelligent macromolecule has extensive research, still, intelligent macromolecule material is used in slow releasing carrier of medication field
Road field is sustained snow melt salt, and there are with high costs, the realistic problems such as complex process.Secondly, being sustained in the materials such as medicament slow release
Dosage is small, and concentration is low, and swelling time is very long, and road field requires salt burst size big, and concentration is high, rate of release after snowing
Fast etc., existing intelligent macromolecule temperature sensing material cannot be met the requirements.
In addition, drug temperature-sensitive sustained release switch temperature is all 30 DEG C or so close to body temperature, and road releases salt and then wishes to release
Salt switch temperature will have low temperature release in 0 DEG C or subzero, the function that high temperature is closed, this considers in material system
When have apparent application characteristic.
Summary of the invention
The technical problems to be solved by the invention: being just released and finished later with salt material rainy season is released for existing road,
The problem of losing snow melting function to winter provides the preparation method that a kind of temperature sensitive type releases salt material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) industrial alkali lignin and deionized water are mixed, carries out magnetic agitation, filtered to get filtrate, be added in filtrate
Potassium sulfate and tetramethylethylenediamine continue 30~40min of stirring to get mixture；
(2) taking mixture, acrylic acid, n-isopropyl acrylamide, acrylamide, mass fraction is 3% formalin, N, and N '-is sub-
Bisacrylamide, dimethoxybenzoin solution, mixture and acrylic acid, n-isopropyl acrylamide, acrylamide are mixed
It closes, carries out magnetic agitation to get mixed liquor A, it is 3% formalin and N, N '-methylene that mass fraction is added in mixed liquor A
Bisacrylamide is stirred to get mixture B, dimethoxybenzoin solution is added in mixed liquid B, stirs evenly,
Reaction solution is obtained, after reaction solution is carried out ultraviolet irradiation processing, is sealed 1 day to get aqueous precursor gel；
(3) aqueous precursor gel is subjected to carrying out washing treatment to get detergent gel, detergent gel is dried to get temperature sensitive
Type releases salt material.
Industrial alkali lignin and deionized water are mixed described in step (1), carry out magnetic stirring process are as follows: in mass ratio
Mix industrial alkali lignin and deionized water at 1: 5,1~2h of magnetic agitation at being 70~80 DEG C in temperature.
The mass ratio of filtrate, potassium peroxydisulfate and tetramethylethylenediamine described in step (1) is 1: 0.2: 0.2.
The preparation step of dimethoxybenzoin solution described in step (2) are as follows: in mass ratio 1: 10 by dimethoxybenzoin
It is uniformly mixed with n-isopropyl acrylamide to get dimethoxybenzoin solution.
Mixture described in step (2), acrylic acid, n-isopropyl acrylamide, acrylamide, mass fraction are 3% formaldehyde
Solution, N, the ratio between N '-methylene-bisacrylamide, dimethoxybenzoin solution are respectively as follows: according to parts by weight, respectively
Weigh 20~30 parts of mixtures, 1~5 part of acrylic acid, 1~10 part of n-isopropyl acrylamide, 1~3 part of acrylamide, 0.3~
0.5 part of mass fraction is 3% formalin, 1~2 part of N, N '-methylene-bisacrylamide, 1~3 part of dimethoxybenzoin solution.
Mixture and acrylic acid, n-isopropyl acrylamide, acrylamide are mixed described in step (2), carry out magnetic force
Whipping step are as follows: mix mixture and acrylic acid, n-isopropyl acrylamide, acrylamide, in the case where temperature is 50~55 DEG C
1~2h of magnetic agitation.
It is 3% formalin and N, N '-methylene bisacrylamide acyl that mass fraction is added described in step (2) in mixed liquor A
Amine is stirred step are as follows: it is 3% formalin and N, N '-methylene bisacrylamide that mass fraction is added in mixed liquor A
Amide stirs 30~50min in the case where revolving speed is 500~600r/min.
Reaction solution is subjected to ultraviolet irradiation processing step described in step (2) are as follows: be in ultraviolet radiation wave-lengths by reaction solution
365nm, power are 6~8h of ultraviolet irradiation under 400W.
Aqueous precursor gel is subjected to carrying out washing treatment step described in step (3) are as follows: aqueous precursor gel is washed with deionized water
It washs 4~5 days, washs 5~6 times daily.
Step is dried in detergent gel described in step (3) are as follows: carry out detergent gel in liquid nitrogen quickly
It freezes, takes out, be placed in freeze drier after 1~2h, be freeze-dried 6~8h at being -40~-50 DEG C in temperature.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention is using industrial alkali lignin as raw material, and formaldehyde and N, N '-methylene-bisacrylamide are crosslinking agent, in over cure
Sour potassium/tetramethylethylenediamine redox system causes lower and acrylic acid, n-isopropyl acrylamide and acrylamide free radical
It is graft-polymerized, the temperature sensitive type for being prepared for a kind of three-dimensional space network crosslinking shape structure releases salt material, and industrial alkali lignin is by benzene
Propane structural unit passes through aromatic polymer polymer made of ehter bond and carbon-carbon bond connection, contains hydroxyl on structural unit
Base, carboxyl and carbonyl isoreactivity group have stronger chelating ability and colloidal property；Persulfate slow-release material is because of its cost
Potentiometric titrations SO cheap, that strong oxidizing property can be generated under the conditions of transition metal-catalyzed4 -, and in acid, neutral, alkali
Good oxidability is all had under the conditions of property；
(2) contain a large amount of phenolic hydroxyl groups and carboxyl in lignin molecule structure, these functional groups are to gold such as calcium, magnesium, copper, iron, zinc, manganese
Belong to member and is known as certain sequestering power；So after alkali lignin is added, due to chemical reaction generation in chelation and film
Reticular structure acts on simultaneously, reaches slow release effect；Acrylic acid is simplest unsaturated carboxylic acid, and molecular chain-end is with high living
Property alkenyl and-COOH group, have efficient reactivity worth and pH sensibility, the addition of acrylic acid and acrylamide, not only
Increase temperature sensitive type and release the biodegradable and bio-compatibility of salt material, and temperature sensitive type can be adjusted release the low of salt material and face
Boundary's solution temperature value；
(3) present invention can be rapidly frozen hydrogel sample by the way of liquid-nitrogen freeze drying, considerably reduce and freezing
With the surface tension effects of drying process hydrone, it can be good at the stability for keeping material structure；High score subclass hydrogel
There are intermolecular hydrogen bonding and intramolecular hydrogen bond in system, when ambient temperature is lower than lower critical solution temperature, hydrogel divides greatly
Hyarogen-bonding between son and hydrone plays a leading role, and solvation between the two is promoted, the water around macromolecular
Molecule forms one layer of regular solvation shell by Hydrogenbond, the hydrone package that hydrophobic group is completely solvated at this time,
Volume expansion occurs at this moment hydrogel water suction, and solvation weakens, and as the temperature rises is destroyed for intermolecular hydrogen bonding, hydrophobic group
Therefore group reveals, the hydrogen bond action of macromolecule internal accounts for leading, hydrogel network generation volume contraction；It will be quick with liquid nitrogen
The hydrogel sample of freezing carries out freeze-drying process, the solvent in wet gel internal void directly from solid state sublimation to gaseous state,
To avoid the appearance of liquid phase, therefore the capillary pressure that can effectively prevent hole drying process from generating, it prevents hole from collapsing, protects
Hold the original structure and morphology of material.
Specific embodiment
In mass ratio 1: 5 mixes industrial alkali lignin and deionized water, and magnetic agitation 1 at being 70~80 DEG C in temperature~
2h filters to get filtrate, and in mass ratio 1: 0.2: 0.2 is added potassium peroxydisulfate and tetramethylethylenediamine in filtrate, continues to stir
30~40min is to get mixture；In mass ratio 1: 10 is uniformly mixed dimethoxybenzoin and n-isopropyl acrylamide, i.e.,
Obtain dimethoxybenzoin solution；According to parts by weight, 20~30 parts of mixtures, 1~5 part of acrylic acid, 1~10 part of N- are weighed respectively
N-isopropylacrylamide, 1~3 part of acrylamide, 0.3~0.5 part of mass fraction are 3% formalin, 1~2 part of N, N '-methylene
Base bisacrylamide, 1~3 part of dimethoxybenzoin solution, by mixture and acrylic acid, n-isopropyl acrylamide, acryloyl
Amine mixing, to get mixed liquor A, mass fraction is added in mixed liquor A is 1~2h of magnetic agitation at being 50~55 DEG C in temperature
3% formalin and N, N '-methylene-bisacrylamide, in the case where revolving speed is 500~600r/min, 30~50min of stirring is to get mixed
Object B is closed, dimethoxybenzoin solution is added in mixed liquid B, stirs evenly, obtains reaction solution, by reaction solution in ultraviolet radioactive wave
A length of 365nm is sealed 1 day after power is 6~8h of ultraviolet irradiation under 400W to get aqueous precursor gel；By aqueous precursor gel
It is washed with deionized 4~5 days, washs 5~6 times daily to get detergent gel, detergent gel is subjected to fast quickly cooling in liquid nitrogen
Freeze, take out, be placed in freeze drier after 1~2h, is freeze-dried 6~8h at being -40~-50 DEG C in temperature to get temperature sensitive
Type releases salt material.
Industrial alkali lignin and deionized water are mixed, magnetic agitation is carried out, filters to get filtrate, is added in filtrate
Potassium peroxydisulfate and tetramethylethylenediamine continue to stir 30min to get mixture；Take mixture, acrylic acid, N- isopropyl propylene
Amide, acrylamide, mass fraction are 3% formalin, N, and N '-methylene-bisacrylamide, dimethoxybenzoin solution will
Mixture and acrylic acid, n-isopropyl acrylamide, acrylamide mixing, carry out magnetic agitation to get mixed liquor A, are mixing
It is 3% formalin and N, N '-methylene-bisacrylamide that mass fraction is added in liquid A, is stirred to get mixture
Dimethoxybenzoin solution is added in mixed liquid B, stirs evenly, obtains reaction solution by B, and reaction solution is carried out ultraviolet irradiation processing
Afterwards, 1 day is sealed to get aqueous precursor gel；Aqueous precursor gel is subjected to carrying out washing treatment to get detergent gel, washing is coagulated
Glue, which is dried, releases salt material to get temperature sensitive type.Industrial alkali lignin and deionized water are mixed, magnetic agitation step is carried out
Suddenly are as follows: in mass ratio 1: 5 mixes industrial alkali lignin and deionized water, magnetic agitation 1h at being 70 DEG C in temperature.Filtrate, mistake
The mass ratio of potassium sulfate and tetramethylethylenediamine is 1: 0.2: 0.2.The preparation step of dimethoxybenzoin solution are as follows: in mass ratio
Be uniformly mixed dimethoxybenzoin and n-isopropyl acrylamide to get dimethoxybenzoin solution at 1: 10.Mixture, propylene
Acid, n-isopropyl acrylamide, acrylamide, mass fraction are 3% formalin, N, and N '-methylene-bisacrylamide is rested in peace
Ratio between fragrant dimethyl ether solution is respectively as follows: according to parts by weight, weighs 20 parts of mixtures, 1 part of acrylic acid, 1 part of N- respectively
N-isopropylacrylamide, 1 part of acrylamide, 0.3 part of mass fraction are 3% formalin, 1 part of N, N '-methylene bisacrylamide acyl
Amine, 1 part of dimethoxybenzoin solution.Mixture and acrylic acid, n-isopropyl acrylamide, acrylamide are mixed, magnetic is carried out
Power whipping step are as follows: mix mixture and acrylic acid, n-isopropyl acrylamide, acrylamide, magnetic at being 50 DEG C in temperature
Power stirs 1h.It is 3% formalin and N, N '-methylene-bisacrylamide that mass fraction is added in mixed liquor A, is stirred
Processing step are as follows: it is 3% formalin and N, N '-methylene-bisacrylamide that mass fraction, which is added, in mixed liquor A, in revolving speed
To stir 30min under 500r/min.Reaction solution is subjected to ultraviolet irradiation processing step are as follows: be in ultraviolet radiation wave-lengths by reaction solution
365nm, power are ultraviolet irradiation 6h under 400W.Aqueous precursor gel is subjected to carrying out washing treatment step are as follows: spend aqueous precursor gel
Ion water washing 4 days, washing 5 times daily.Step is dried in detergent gel are as follows: carry out detergent gel in liquid nitrogen
It is rapidly frozen, takes out, be placed in freeze drier after 1h, be freeze-dried 6h at being -40 DEG C in temperature.
Industrial alkali lignin and deionized water are mixed, magnetic agitation is carried out, filters to get filtrate, is added in filtrate
Potassium peroxydisulfate and tetramethylethylenediamine continue to stir 35min to get mixture；Take mixture, acrylic acid, N- isopropyl propylene
Amide, acrylamide, mass fraction are 3% formalin, N, and N '-methylene-bisacrylamide, dimethoxybenzoin solution will
Mixture and acrylic acid, n-isopropyl acrylamide, acrylamide mixing, carry out magnetic agitation to get mixed liquor A, are mixing
It is 3% formalin and N, N '-methylene-bisacrylamide that mass fraction is added in liquid A, is stirred to get mixture
Dimethoxybenzoin solution is added in mixed liquid B, stirs evenly, obtains reaction solution by B, and reaction solution is carried out ultraviolet irradiation processing
Afterwards, 1 day is sealed to get aqueous precursor gel；Aqueous precursor gel is subjected to carrying out washing treatment to get detergent gel, washing is coagulated
Glue, which is dried, releases salt material to get temperature sensitive type.Industrial alkali lignin and deionized water are mixed, magnetic agitation step is carried out
Suddenly are as follows: in mass ratio 1: 5 mixes industrial alkali lignin and deionized water, magnetic agitation 1.5h at being 75 DEG C in temperature.Filtrate,
The mass ratio of potassium peroxydisulfate and tetramethylethylenediamine is 1: 0.2: 0.2.The preparation step of dimethoxybenzoin solution are as follows: press quality
Dimethoxybenzoin and n-isopropyl acrylamide are uniformly mixed to get dimethoxybenzoin solution than 1: 10.Mixture, third
Olefin(e) acid, n-isopropyl acrylamide, acrylamide, mass fraction are 3% formalin, N, N '-methylene-bisacrylamide, peace
The ratio ceased between fragrant dimethyl ether solution is respectively as follows: according to parts by weight, weighs 25 parts of mixtures, 3 parts of acrylic acid, 5 parts respectively
N-isopropyl acrylamide, 2 parts of acrylamides, 0.4 part of mass fraction are 3% formalin, 1.5 parts of N, N '-methylene bisacrylamide
Amide, 2 parts of dimethoxybenzoin solution.Mixture and acrylic acid, n-isopropyl acrylamide, acrylamide are mixed, carried out
Magnetic stirring process are as follows: mix mixture and acrylic acid, n-isopropyl acrylamide, acrylamide, in the case where temperature is 53 DEG C
Magnetic agitation 1.5h.It is 3% formalin and N, N '-methylene-bisacrylamide that mass fraction is added in mixed liquor A, is carried out
Stir process step are as follows: in mixed liquor A be added mass fraction be 3% formalin and N, N '-methylene-bisacrylamide,
Revolving speed is to stir 40min under 55r/min.Reaction solution is subjected to ultraviolet irradiation processing step are as follows: by reaction solution in ultraviolet radioactive wave
A length of 365nm, power are ultraviolet irradiation 7h under 400W.Aqueous precursor gel is subjected to carrying out washing treatment step are as follows: by aqueous precursor gel
It is washed with deionized 4.5 days, daily washing 5 times.Step is dried in detergent gel are as follows: by detergent gel in liquid nitrogen
In be rapidly frozen, take out, be placed in freeze drier after 1.5h, temperature be -45 DEG C at be freeze-dried 7h.
Industrial alkali lignin and deionized water are mixed, magnetic agitation is carried out, filters to get filtrate, is added in filtrate
Potassium peroxydisulfate and tetramethylethylenediamine continue to stir 40min to get mixture；Take mixture, acrylic acid, N- isopropyl propylene
Amide, acrylamide, mass fraction are 3% formalin, N, and N '-methylene-bisacrylamide, dimethoxybenzoin solution will
Mixture and acrylic acid, n-isopropyl acrylamide, acrylamide mixing, carry out magnetic agitation to get mixed liquor A, are mixing
It is 3% formalin and N, N '-methylene-bisacrylamide that mass fraction is added in liquid A, is stirred to get mixture
Dimethoxybenzoin solution is added in mixed liquid B, stirs evenly, obtains reaction solution by B, and reaction solution is carried out ultraviolet irradiation processing
Afterwards, 1 day is sealed to get aqueous precursor gel；Aqueous precursor gel is subjected to carrying out washing treatment to get detergent gel, washing is coagulated
Glue, which is dried, releases salt material to get temperature sensitive type.Industrial alkali lignin and deionized water are mixed, magnetic agitation step is carried out
Suddenly are as follows: in mass ratio 1: 5 mixes industrial alkali lignin and deionized water, magnetic agitation 2h at being 80 DEG C in temperature.Filtrate, mistake
The mass ratio of potassium sulfate and tetramethylethylenediamine is 1: 0.2: 0.2.The preparation step of dimethoxybenzoin solution are as follows: in mass ratio
Be uniformly mixed dimethoxybenzoin and n-isopropyl acrylamide to get dimethoxybenzoin solution at 1: 10.Mixture, propylene
Acid, n-isopropyl acrylamide, acrylamide, mass fraction are 3% formalin, N, and N '-methylene-bisacrylamide is rested in peace
Ratio between fragrant dimethyl ether solution is respectively as follows: according to parts by weight, weighs 30 parts of mixtures, 5 parts of acrylic acid, 10 parts of N- respectively
N-isopropylacrylamide, 3 parts of acrylamides, 0.5 part of mass fraction are 3% formalin, 2 parts of N, N '-methylene bisacrylamide acyl
Amine, 3 parts of dimethoxybenzoin solution.Mixture and acrylic acid, n-isopropyl acrylamide, acrylamide are mixed, magnetic is carried out
Power whipping step are as follows: mix mixture and acrylic acid, n-isopropyl acrylamide, acrylamide, magnetic at being 55 DEG C in temperature
Power stirs 2h.It is 3% formalin and N, N '-methylene-bisacrylamide that mass fraction is added in mixed liquor A, is stirred
Processing step are as follows: it is 3% formalin and N, N '-methylene-bisacrylamide that mass fraction, which is added, in mixed liquor A, in revolving speed
To stir 50min under 600r/min.Reaction solution is subjected to ultraviolet irradiation processing step are as follows: be in ultraviolet radiation wave-lengths by reaction solution
365nm, power are ultraviolet irradiation 8h under 400W.Aqueous precursor gel is subjected to carrying out washing treatment step are as follows: spend aqueous precursor gel
Ion water washing 5 days, washing 6 times daily.Step is dried in detergent gel are as follows: carry out detergent gel in liquid nitrogen
It is rapidly frozen, takes out, be placed in freeze drier after 2h, be freeze-dried 8h at being -50 DEG C in temperature.
Temperature sensitive type prepared by the present invention is released into salt material and commercially available snow melting material detects, specific testing result is as follows
Table table 1:
Test method:
Take that 10 grams of finely ground example 1-3 temperature sensitive types release salt material and comparative example evenly spreads to and fills 20 grams 150 DEG C of 70# asphaltic liquid
In body container, after cooling, it be added in 150 ml deionized waters and measure chloride ion precipitation concentration at 0 DEG C and 30 DEG C respectively
1 temperature sensitive type of table releases salt material performance characterization
Temperature sensitive type prepared by the present invention releases salt material as shown in Table 1, and temperature sensitive performance is good, releases salt temperature and concentration is existing market institute
Product in need, has a vast market value and application prospect.
Claims (10)
1. the preparation method that a kind of temperature sensitive type releases salt material, it is characterised in that specific preparation step are as follows:
(1) industrial alkali lignin and deionized water are mixed, carries out magnetic agitation, filtered to get filtrate, be added in filtrate
Potassium sulfate and tetramethylethylenediamine continue 30~40min of stirring to get mixture；
(2) taking mixture, acrylic acid, n-isopropyl acrylamide, acrylamide, mass fraction is 3% formalin, N, and N '-is sub-
Bisacrylamide, dimethoxybenzoin solution, mixture and acrylic acid, n-isopropyl acrylamide, acrylamide are mixed
It closes, carries out magnetic agitation to get mixed liquor A, it is 3% formalin and N, N '-methylene that mass fraction is added in mixed liquor A
Bisacrylamide is stirred to get mixture B, dimethoxybenzoin solution is added in mixed liquid B, stirs evenly,
Reaction solution is obtained, after reaction solution is carried out ultraviolet irradiation processing, is sealed 1 day to get aqueous precursor gel；
(3) aqueous precursor gel is subjected to carrying out washing treatment to get detergent gel, detergent gel is dried to get temperature sensitive
Type releases salt material.
2. the preparation method that a kind of temperature sensitive type according to claim 1 releases salt material, it is characterised in that: step (1) is described
Industrial alkali lignin and deionized water are mixed, carry out magnetic stirring process are as follows: in mass ratio 1: 5 by industrial alkali lignin and
Deionized water mixing, 1~2h of magnetic agitation at being 70~80 DEG C in temperature.
3. the preparation method that a kind of temperature sensitive type according to claim 1 releases salt material, it is characterised in that: step (1) is described
Filtrate, potassium peroxydisulfate and tetramethylethylenediamine mass ratio be 1: 0.2: 0.2.
4. the preparation method that a kind of temperature sensitive type according to claim 1 releases salt material, it is characterised in that: step (2) is described
Dimethoxybenzoin solution preparation step are as follows: in mass ratio 1: 10 mixes dimethoxybenzoin and n-isopropyl acrylamide
It closes uniformly to get dimethoxybenzoin solution.
5. the preparation method that a kind of temperature sensitive type according to claim 1 releases salt material, it is characterised in that: step (2) is described
Mixture, acrylic acid, n-isopropyl acrylamide, acrylamide, mass fraction be 3% formalin, N, N '-di-2-ethylhexylphosphine oxide
Ratio between acrylamide, dimethoxybenzoin solution is respectively as follows: according to parts by weight, weighs 20~30 parts of mixing respectively
Object, 1~5 part of acrylic acid, 1~10 part of n-isopropyl acrylamide, 1~3 part of acrylamide, 0.3~0.5 part of mass fraction are 3%
Formalin, 1~2 part of N, N '-methylene-bisacrylamide, 1~3 part of dimethoxybenzoin solution.
6. the preparation method that a kind of temperature sensitive type according to claim 1 releases salt material, it is characterised in that: step (2) is described
Mixture and acrylic acid, n-isopropyl acrylamide, acrylamide are mixed, carry out magnetic stirring process are as follows: by mixture
With acrylic acid, n-isopropyl acrylamide, acrylamide mixing, 1~2h of magnetic agitation at being 50~55 DEG C in temperature.
7. the preparation method that a kind of temperature sensitive type according to claim 1 releases salt material, it is characterised in that: step (2) is described
In mixed liquor A be added mass fraction be 3% formalin and N, N '-methylene-bisacrylamide, be stirred step
Are as follows: in mixed liquor A be added mass fraction be 3% formalin and N, N '-methylene-bisacrylamide, revolving speed be 500~
30~50min is stirred under 600r/min.
8. the preparation method that a kind of temperature sensitive type according to claim 1 releases salt material, it is characterised in that: step (2) is described
Reaction solution is subjected to ultraviolet irradiation processing step are as follows: by reaction solution in ultraviolet radiation wave-lengths be 365nm, power is purple under 400W
6~8h of external exposure.
9. the preparation method that a kind of temperature sensitive type according to claim 1 releases salt material, it is characterised in that: step (3) is described
Aqueous precursor gel is subjected to carrying out washing treatment step are as follows: aqueous precursor gel is washed with deionized 4~5 days, wash 5 daily~
6 times.
10. the preparation method that a kind of temperature sensitive type according to claim 1 releases salt material, it is characterised in that: step (3) is described
Step is dried in detergent gel are as follows: detergent gel is rapidly frozen in liquid nitrogen, is taken out after 1~2h, and
It is placed in freeze drier, is freeze-dried 6~8h at being -40~-50 DEG C in temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112999119A (en) * | 2021-03-24 | 2021-06-22 | 蒋涛 | Gel-like cosmetic with lasting moisturizing function and preparation method thereof |
| CN113308226A (en) * | 2021-06-07 | 2021-08-27 | 绍兴徐越环境服务有限公司 | Pavement humectant and preparation method thereof |
-
2019
- 2019-03-02 CN CN201910157715.0A patent/CN109970929A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112999119A (en) * | 2021-03-24 | 2021-06-22 | 蒋涛 | Gel-like cosmetic with lasting moisturizing function and preparation method thereof |
| CN113308226A (en) * | 2021-06-07 | 2021-08-27 | 绍兴徐越环境服务有限公司 | Pavement humectant and preparation method thereof |
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