CN108047377A - A kind of temperature-sensitive hydrogel and preparation method thereof - Google Patents
A kind of temperature-sensitive hydrogel and preparation method thereof Download PDFInfo
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- CN108047377A CN108047377A CN201711273647.1A CN201711273647A CN108047377A CN 108047377 A CN108047377 A CN 108047377A CN 201711273647 A CN201711273647 A CN 201711273647A CN 108047377 A CN108047377 A CN 108047377A
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
- A62D1/0064—Gels; Film-forming compositions
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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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
- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
- C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
- C08F290/06—Polymers provided for in subclass C08G
- C08F290/062—Polyethers
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Abstract
The invention discloses a kind of temperature-sensitive hydrogels and preparation method thereof, belong to technical field of hydrogel.The preparation method of the hydrogel comprises the following steps：(1) it is configured to reaction solution with methylcellulose and deionized water；(2) by the use of above-mentioned reaction solution as solvent, it is each configured to NaHCO3Solution and NaOH solution, then by NaHCO3Acid base titration is carried out to a certain amount of acrylic acid with it after solution and NaOH solution mixing, the sodium acrylate monomers that pH value is 7.0 is obtained and adjusts liquid；(3) N N-isopropylacrylamides are added in into four-hole bottle by a certain percentage, under conditions of nitrogen protection, a certain amount of sodium acrylate monomers adjustment liquid is slowly added dropwise into four-hole bottle, obtains lysate；(4) crosslinking agent, initiator and catalyst are added in above-mentioned lysate, temperature-sensitive hydrogel is made.The temperature-sensitive hydrogel of the present invention has good extinguishing property.
Description
Technical field
The present invention relates to technical field of hydrogel, and in particular to a kind of temperature-sensitive hydrogel and preparation method thereof.
Background technology
Water is current most common extinguishing chemical.In recent years, researcher is done in terms of how improving the fire-fighting efficiency of water
Substantial amounts of innovative works are mainly manifested in and add different chemical reagent in water or change the physicochemical characteristic of water to increase
The viscosity and adhesive force of strong water extend water retention time in combustion zone, improve effective oxygen barrier cooling capacity of water, using water wisely
Amount to give full play to the extinguishing property of water, improves fire-fighting efficiency.Current research it is most have water mists, three-phase froth, MJPZ
The water-based extinguishing agents such as foam and hydrogel.Hydrogel extinguishing chemical can improve viscosity and adhesive force of the water in body surface, enhancing
Solid water, closure, isolation and the cooling effect of water, it has also become one of domestic and international research hotspot.
The volume energy of temperature-sensitive hydrogel changes with the variation of environment temperature, and intramolecular has a certain proportion of hydrophobic
And hydrophilic radical, when environment temperature is in its lower critical solution temperature (LCST, Lower Critical Solution
When minor variations Temperature) nearby occur, affect the hydrogen bond action between the hydrophobic effect of group, macromolecular chain with
And discontinuous phase transformation or sol/gel transformation can occur for the hydrogen bond action between hydrophilic radical, temperature-sensitive hydrogel.It is temperature sensitive
Property hydrogel has two kinds of heat expansion type and thermal shrinkage type.The swellbility of heat expansion type hydrogel is raised with the rise of temperature, in high temperature
Lower macromolecular chain Quick extension due to aquation；Thermal shrinkage type hydrogel in higher temperature macromolecular chain because aggregation
And shrink, swellbility also drastically declines therewith, but can be then swollen at present than relatively low temperature.Poly-N-isopropyl acryloyl
Aqueous amine gel is current most study, it belongs to typical thermal shrinkage type hydrogel, and volume discontinuities can occur at 32 DEG C or so.
In recent years, temperature-sensitive hydrogel is still in exploration stage as the application of fire-extinguishing chemical.Due to its preparative separation
Complex process, cost is higher, therefore current is difficult to be widely popularized and apply.There is presently no develop the temperature sensitive of special efficacy both at home and abroad
It, can be equipped fire department above county level and emergency management and rescue unit extensively by property hydrogel extinguishing chemical after researching and developing successfully.The application
The production technology of temperature-sensitive hydrogel extinguishing chemical is studied, so as to effectively reduce extinguishing chemical cost, makes temperature-sensitive hydrogel
Extinguishing chemical is converted from theoretical research to practical application.The development of efficient temperature-sensitive hydrogel extinguishing chemical can effectively fill up domestic
The blank in the outer field.
The content of the invention
In view of the above-mentioned problems, the present invention will use the method being freely copolymerized by n-isopropyl acrylamide and acrylic acid with one
Certainty ratio synthesizes temperature-sensitive hydrogel under the action of initiator and is used as extinguishing chemical, passes through pair with ordinary gel
Than experiment, which has efficient fire extinguishing effect.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of preparation method of temperature-sensitive hydrogel, comprises the following steps：
(1) to be pre-configured to the reaction that concentration is 39%-41% with methylcellulose and 75 DEG C of -85 DEG C of deionized waters molten
After being sufficiently stirred, it is for use to be put into standing 55h-65h in refrigerator for liquid；
(2) by the use of above-mentioned reaction solution as solvent, NaHCO3 solution and NaOH that concentration is 2mol/L are each configured to
Solution carries out acid base titration to a certain amount of acrylic acid with it after then mixing NaHCO3 solution and NaOH solution, obtains PH
It is worth and adjusts liquid for 7.0 sodium acrylate monomers；
(3) n-isopropyl acrylamide is added in into the four-hole bottle of 1000ml by a certain percentage, in the condition of nitrogen protection
Under, a certain amount of sodium acrylate monomers adjustment liquid is slowly added dropwise into four-hole bottle, mechanical agitation is dissolved to abundant dissolving
Liquid；
(4) the crosslinking agent 0.9ml-1.1ml that mass fraction is 10% is added in above-mentioned lysate, adds mass fraction
The catalyst 1.9ml-2.1ml that initiator 0.9ml-1.1ml and addition mass fraction for 10% are 10%, at 24 DEG C -26
22~26h is reacted at a temperature of DEG C, required temperature-sensitive hydrogel is made.
Preferably, it is additionally included in after step (4) and again product is carried out to rinse 2-3 times repeatedly, afterwards in 65 DEG C of -75 DEG C of temperature
Lower vacuum drying 46h-50h, it is spare to be ground into white powder.
Preferably, product is rinsed repeatedly using swelling shrinkage method.
Preferably, in the step (3), the ratio between amount of substance of n-isopropyl acrylamide and sodium acrylate is 10:1.
Preferably, in the step (3), mixing time 15-25min.
Preferably, in the step (4), initiator is one or both of ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate
More than.
Preferably, in the step (4), catalyst N, N, N ', N '-tetramethylethylenediamine aqueous solution, triethanolamine, sulphur
One kind in sodium thiosulfate.
Preferably, in the step (4), crosslinking agent N, N '-methylene-bisacrylamide, polyethylene glycol diacrylate
It is more than one or both of ester, polyethylene glycol dimethacrylate.
Present invention additionally comprises the temperature-sensitive hydrogels that the preparation method of the temperature-sensitive hydrogel is prepared.
In conclusion by adopting the above-described technical solution, beneficial effects of the present invention are：
The temperature-sensitive hydrogel that the present invention is prepared, either by its alone as extinguishing chemical still by its with
Water is combined collectively as extinguishing chemical, can play the role of good fire extinguishing.Turn because sol/gel can occur for temperature-sensitive hydrogel
Become, in fire extinguishing procedure, temperature-sensitive hydrogel generates foam-like gel due to high temperature, can increase the viscosity of extinguishing chemical, be conducive to
Temperature-sensitive hydrogel is adsorbed on combustible object surface, and then improves residence time and stop of the extinguishing chemical on combustible substance surface
Amount so as to improve the cooling of extinguishing chemical and plugging effect, is finally reached efficient fire extinguishing effect.
In conclusion energy rapid osmotic is coagulated again to interior of articles after temperature-sensitive hydrogel is ejected into the object that catches fire as extinguishing chemical
Adhesive curing forms a film, and to achieve the effect that most effective fire extinguishing, prevents resume combustion.
Specific embodiment
The technical solution in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only part of the embodiment of the present invention, instead of all the embodiments.
Embodiment 1
A kind of preparation method of temperature-sensitive hydrogel, comprises the following steps：
(1) reaction solution that concentration is 39% is pre-configured to methylcellulose and 75 DEG C of deionized waters, be sufficiently stirred
Afterwards, it is for use to be put into standing 55h in refrigerator；
(2) by the use of above-mentioned reaction solution as solvent, it is each configured to the NaHCO that concentration is 2mol/L3Solution and NaOH
Solution, then by NaHCO3Acid base titration is carried out to a certain amount of acrylic acid with it after solution and NaOH solution mixing, obtains PH
It is worth and adjusts liquid for 7.0 sodium acrylate monomers；Wherein, methylcellulose can preferably form thickening power with acrylic acid；
(3) n-isopropyl acrylamide is added in into the four-hole bottle of 1000ml by a certain percentage, in the condition of nitrogen protection
Under, it is slowly added dropwise a certain amount of sodium acrylate monomers adjustment liquid into four-hole bottle, n-isopropyl acrylamide and sodium acrylate
The ratio between amount of substance is 10:1, mechanical agitation 15min obtain lysate to abundant dissolving；
(4) the crosslinking agent 0.9ml that mass fraction is 10% is added in above-mentioned lysate, adds mass fraction as 10%
Initiator 0.9ml and add in mass fraction be 10% catalyst 1.9ml, react 26h at a temperature of 24 DEG C, obtain
Product；Then product is carried out again using swelling shrinkage method to rinse 2 times repeatedly, is dried in vacuo 50h, powder at a temperature of 65 DEG C afterwards
It is broken into that white powder is spare, required temperature-sensitive hydrogel is made.Wherein, initiator is ammonium persulfate, and catalyst is three ethyl alcohol
Amine, crosslinking agent N, N '-methylene-bisacrylamide.
Present invention additionally comprises the temperature-sensitive hydrogels that the preparation method of the temperature-sensitive hydrogel is prepared.
Embodiment 2
A kind of preparation method of temperature-sensitive hydrogel, comprises the following steps：
(1) reaction solution that concentration is 40% is pre-configured to methylcellulose and 80 DEG C of deionized waters, be sufficiently stirred
Afterwards, it is for use to be put into standing 60h in refrigerator；
(2) by the use of above-mentioned reaction solution as solvent, it is each configured to the NaHCO that concentration is 2mol/L3Solution and NaOH
Solution, then by NaHCO3Acid base titration is carried out to a certain amount of acrylic acid with it after solution and NaOH solution mixing, obtains PH
It is worth and adjusts liquid for 7.0 sodium acrylate monomers；Wherein, methylcellulose can preferably form thickening power with acrylic acid；
(3) n-isopropyl acrylamide is added in into the four-hole bottle of 1000ml by a certain percentage, in the condition of nitrogen protection
Under, it is slowly added dropwise a certain amount of sodium acrylate monomers adjustment liquid into four-hole bottle, n-isopropyl acrylamide and sodium acrylate
The ratio between amount of substance is 10:1, mechanical agitation 20min obtain lysate to abundant dissolving；
(4) the crosslinking agent 1ml that mass fraction is 10% is added in above-mentioned lysate, it is 10% to add mass fraction
The catalyst 2ml that initiator 1ml and addition mass fraction are 10%, reacts for 24 hours at a temperature of 25 DEG C, obtains product；So
Afterwards product is carried out again using swelling shrinkage method to rinse 3 times repeatedly, be dried in vacuo 48h at a temperature of 70 DEG C afterwards, be ground into white
Color powder is spare, and required temperature-sensitive hydrogel is made.Wherein, initiator be ammonium persulfate and sodium peroxydisulfate, catalyst N,
N, N ', N '-tetramethylethylenediamine aqueous solution, crosslinking agent N, N '-methylene-bisacrylamide and polyethyleneglycol diacrylate.
Present invention additionally comprises the temperature-sensitive hydrogels that the preparation method of the temperature-sensitive hydrogel is prepared.
Embodiment 3
A kind of preparation method of temperature-sensitive hydrogel, comprises the following steps：
(1) reaction solution that concentration is 41% is pre-configured to methylcellulose and 85 DEG C of deionized waters, be sufficiently stirred
Afterwards, it is for use to be put into standing 65h in refrigerator；
(2) by the use of above-mentioned reaction solution as solvent, it is each configured to the NaHCO that concentration is 2mol/L3Solution and NaOH
Solution, then by NaHCO3Acid base titration is carried out to a certain amount of acrylic acid with it after solution and NaOH solution mixing, obtains PH
It is worth and adjusts liquid for 7.0 sodium acrylate monomers；Wherein, methylcellulose can preferably form thickening power with acrylic acid；
(3) n-isopropyl acrylamide is added in into the four-hole bottle of 1000ml by a certain percentage, in the condition of nitrogen protection
Under, it is slowly added dropwise a certain amount of sodium acrylate monomers adjustment liquid into four-hole bottle, n-isopropyl acrylamide and sodium acrylate
The ratio between amount of substance is 10:1, mechanical agitation 25min obtain lysate to abundant dissolving；
(4) the crosslinking agent 1.1ml that mass fraction is 10% is added in above-mentioned lysate, adds mass fraction as 10%
Initiator 1.1ml and add in mass fraction be 10% catalyst 2.1ml, react 22h at a temperature of 26 DEG C, obtain
Product；Then product is carried out again using swelling shrinkage method to rinse 3 times repeatedly, is dried in vacuo 46h, powder at a temperature of 75 DEG C afterwards
It is broken into that white powder is spare, required temperature-sensitive hydrogel is made.Wherein, initiator is ammonium persulfate, sodium peroxydisulfate and over cure
Sour potassium, catalyst are sodium thiosulfate, crosslinking agent N, N '-methylene-bisacrylamide, polyethyleneglycol diacrylate and poly-
Ethylene glycol dimethacrylate.
Present invention additionally comprises the temperature-sensitive hydrogels that the preparation method of the temperature-sensitive hydrogel is prepared.
The applicant has done substantial amounts of development test to the extinguishing property of temperature-sensitive hydrogel, now arranges part test such as
Under：
Applicant's simulated fire establishes fiery experimental model, and experiment sets 4 test groups altogether, and each test group sets an oil
Disk adds in the diesel oil of equivalent in each food tray, is then ignited with cotton yarn, start to spray after the diesel combustion 3min on food tray
Penetrate extinguishing chemical：
1st group：It is put out a fire using the temperature-sensitive hydrogel in the present embodiment 1 as extinguishing chemical；
2nd group：It is put out a fire using the temperature-sensitive hydrogel in the present embodiment 2 as extinguishing chemical；
3rd group：It is put out a fire using the temperature-sensitive hydrogel in the present embodiment 3 as extinguishing chemical；
4th group：It is put out a fire using common hydrogel as extinguishing chemical.
The situation of fray-out of flame is observed and recorded in fire extinguishing procedure, is counted each data, is as a result counted as shown in table 1 below.
Each achievement data of 1 fire extinguishing procedure of table
| Grouping | Peak flame temperature/DEG C | Temperature is down to 200 DEG C of used time/s | Whether there is resume combustion |
| 1st group | 664 | 37 | Nothing |
| 2nd group | 665 | 35 | Nothing |
| 3rd group | 663 | 36 | Nothing |
| 4th group | 665 | 120 | Have |
From the results shown in Table 1, when doing fire-extinguishing test, the 1st group, the 2nd group and the 3rd group is synthesized using the application
Temperature-sensitive hydrogel put out a fire, experienced three phases during the food tray fire that goes out：First, pre-combustion period, food tray
It is ignited simultaneously vigorous combustion；Second is that since fire phases, be all extinguished starting spray fire extinguishing agent to food tray flame；Third, it goes out
Refiring after fire after putting out a fire, pushes the temperature-sensitive hydrogel of sump pan surface aside, can rekindle food tray, it was demonstrated that go out
Fire is successful.After fire extinguishing terminates, it can be seen that after the temperature-sensitive hydrogel fire extinguishing of synthesis, occur one layer in vain in sump pan surface
The foam-like gel of color, these gels are densely floated on pasta, can effectively be completely cut off air, therefore can effectively be put out food tray
Fire.And the 4th group as extinguishing chemical due to being put out a fire using common hydrogel, because of common hydrogel, not possess generation molten
The performance of glue/gel conversion, therefore do not have fire extinguishing effect.
Claims (9)
1. a kind of preparation method of temperature-sensitive hydrogel, which is characterized in that comprise the following steps：
(1) reaction solution that concentration is 39%-41% is pre-configured to methylcellulose and 75 DEG C of -85 DEG C of deionized waters, filled
After dividing stirring, it is for use to be put into standing 55h-65h in refrigerator；
(2) by the use of above-mentioned reaction solution as solvent, it is each configured to the NaHCO that concentration is 2mol/L3Solution and NaOH solution,
Then by NaHCO3Acid base titration is carried out to a certain amount of acrylic acid with it after solution and NaOH solution mixing, obtaining pH value is
7.0 sodium acrylate monomers adjustment liquid；
(3) n-isopropyl acrylamide is added in into the four-hole bottle of 1000ml by a certain percentage, under conditions of nitrogen protection, to
A certain amount of sodium acrylate monomers adjustment liquid is slowly added dropwise in four-hole bottle, mechanical agitation obtains lysate to abundant dissolving；
(4) the crosslinking agent 0.9ml-1.1ml that mass fraction is 10% is added in above-mentioned lysate, adding mass fraction is
The catalyst 1.9ml-2.1ml that 10% initiator 0.9ml-1.1ml and addition mass fraction is 10%, at 24 DEG C -26 DEG C
At a temperature of react 22~26h, required temperature-sensitive hydrogel is made.
2. the preparation method of temperature-sensitive hydrogel according to claim 1, which is characterized in that after being additionally included in step (4)
Product is carried out again to rinse 2-3 times repeatedly, 46h-50h is dried in vacuo at a temperature of 65 DEG C -75 DEG C afterwards, is ground into white powder
It is spare.
3. the preparation method of temperature-sensitive hydrogel according to claim 2, which is characterized in that using swelling shrinkage method to production
Object is rinsed repeatedly.
4. the preparation method of temperature-sensitive hydrogel according to claim 1, which is characterized in that in the step (3), N- is different
The ratio between amount of substance of propylacrylamide and sodium acrylate is 10:1.
5. the preparation method of temperature-sensitive hydrogel according to claim 1, which is characterized in that in the step (3), stirring
Time is 15-25min.
6. the preparation method of temperature-sensitive hydrogel according to claim 1, which is characterized in that in the step (4), trigger
Agent is more than one or both of ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate.
7. the preparation method of temperature-sensitive hydrogel according to claim 1, which is characterized in that in the step (4), catalysis
Agent is N, N, N ', one kind in N '-tetramethylethylenediamine aqueous solution, triethanolamine, sodium thiosulfate.
8. the preparation method of temperature-sensitive hydrogel according to claim 1, which is characterized in that in the step (4), crosslinking
Agent is N, one kind in N '-methylene-bisacrylamide, polyethyleneglycol diacrylate, polyethylene glycol dimethacrylate or
It is two or more.
9. a kind of Thermo-sensitive water that preparation method according to claim 1-8 any one of them temperature-sensitive hydrogels is prepared
Gel.
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Cited By (8)
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| CN110156926A (en) * | 2019-06-04 | 2019-08-23 | 北京理工大学 | Low-density foamed hydrogel pad and preparation method thereof, extinguishing device |
| CN110404225A (en) * | 2019-08-26 | 2019-11-05 | 西安科技大学 | A kind of environment-friendly type macromolecule colloid extinguishment additive agent and its preparation method and application |
| CN110478845A (en) * | 2019-09-11 | 2019-11-22 | 江西科技师范大学 | A kind of cellulose base hydrogel extinguishing chemical and the preparation method and application thereof with height water-retaining property |
| CN111635480A (en) * | 2020-06-29 | 2020-09-08 | 苏州凝智新材料发展有限公司 | Anti-swelling hydrogel material and preparation method thereof |
| CN111992037A (en) * | 2019-05-27 | 2020-11-27 | 宝山钢铁股份有限公司 | Forward osmosis hydrogel draw solution, preparation method and application 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 |
| CN113388068A (en) * | 2020-03-11 | 2021-09-14 | 中国石油化工股份有限公司 | Cooling and heat insulating material composition based on temperature-sensitive gel, cooling and heat insulating material based on temperature-sensitive gel and application thereof |
| CN114479122A (en) * | 2022-01-20 | 2022-05-13 | 西南石油大学 | Biomass hydrogel, preparation method and application |
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| CN114479122A (en) * | 2022-01-20 | 2022-05-13 | 西南石油大学 | Biomass hydrogel, preparation method and application |
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