CN109232958A - A kind of preparation method of porous aquagel - Google Patents

A kind of preparation method of porous aquagel Download PDF

Info

Publication number
CN109232958A
CN109232958A CN201810727061.6A CN201810727061A CN109232958A CN 109232958 A CN109232958 A CN 109232958A CN 201810727061 A CN201810727061 A CN 201810727061A CN 109232958 A CN109232958 A CN 109232958A
Authority
CN
China
Prior art keywords
parts
preparation
porous aquagel
polyvinyl alcohol
acrylamide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201810727061.6A
Other languages
Chinese (zh)
Inventor
雷国平
兰梅菊
吴庆梅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changzhou Oman Medical Science And Technology Co Ltd
Original Assignee
Changzhou Oman Medical Science And Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Changzhou Oman Medical Science And Technology Co Ltd filed Critical Changzhou Oman Medical Science And Technology Co Ltd
Priority to CN201810727061.6A priority Critical patent/CN109232958A/en
Publication of CN109232958A publication Critical patent/CN109232958A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/08Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0014Use of organic additives
    • C08J9/0023Use of organic additives containing oxygen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0061Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0066Use of inorganic compounding ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0095Mixtures of at least two compounding ingredients belonging to different one-dot groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00Foams characterized by the expanding agent
    • C08J2203/02CO2-releasing, e.g. NaHCO3 and citric acid
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2333/00Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2333/24Homopolymers or copolymers of amides or imides
    • C08J2333/26Homopolymers or copolymers of acrylamide or methacrylamide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2429/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2429/02Homopolymers or copolymers of unsaturated alcohols
    • C08J2429/04Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2489/00Characterised by the use of proteins; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2491/00Characterised by the use of oils, fats or waxes; Derivatives thereof

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Emergency Medicine (AREA)
  • Colloid Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of preparation methods of porous aquagel, belong to technical field of polymer materials.The present invention according to parts by weight, successively takes 40~50 parts of pretreatment acrylamides, 8~10 parts of drying oil, 3~5 parts of linoleic acid, 5~8 parts of emulsifiers, 8~10 parts of calcium carbonate, 2~3 parts of ammonium persulfates, 10~20 parts of modified additives, 8~10 parts of composite foamable agents, 60~80 parts of water;Acrylamide, drying oil, linoleic acid, emulsifier, calcium carbonate and water mixing will be pre-processed, ammonium persulfate is subsequently added into, the reaction of nitrogen charging heating stirring is subsequently added into modified additive and composite foamable agent, and injection molding is stood, and demoulding obtains blank;Blank is placed in ultrasonic immersing in hydrochloric acid, is taken out, it is dry to get porous aquagel.The porous aquagel of technical solution of the present invention preparation has the characteristics that porosity and intensity are high, has broad prospects in the development of high polymer material technology industry.

Description

A kind of preparation method of porous aquagel
Technical field
The invention discloses a kind of preparation methods of porous aquagel, belong to technical field of polymer materials.
Background technique
Hydrogel is a kind of hydrophily but high molecular polymer not soluble in water.It is flat that they can be swelling to rapidly one in water Weighing apparatus volume and be still able to maintain its shape and three-dimensional space network structure, and be dehydrated deswelling under certain conditions, be a class set Water suction, is sustained in one and the functional polymer material that quickly grows water conservation.Because its is unique, water conservation and bionical characteristic, water Gel is widely used in the purposes of industry, agricultural, medicine and biological engineering material field hydrogel mainly by swelling rate, molten The parameters such as swollen rate and mechanical strength characterize.Although the gel of conventional method synthesis can obtain higher swelling ratio, its is molten Swollen dynamics is usually all relatively slow, is influenced by material selection and production technology, the swelling of hydrogel and deswelling time can From several seconds to even a few days a few hours.In practical application, generally the swelling rate of hydrogel need to be improved by reducing size, this Just hydrogel is significantly limited in the application of the fields of biomedicine such as medicine controlled releasing, transmission and organizational project.It is solidifying in order to get rid of Limitation of the glue size to the swelling deswelling rate of hydrogel extends it and is needing quick response rate field, especially as Use in terms of enviromental sensitive hydrogel, it is a kind of effective method in porous water that porous structure is introduced into hydrogel In gel, the scale calibration for determining swelling time is pitch of holes rather than gel three-dimensional size.When diffusion path narrows down to enough Short (capillary channel), and between hole be it is interconnected, the transfer rate of swelling solution will primarily depend upon capillary force, compared with Its diffusion process in polymer network is much faster.Therefore, the swelling that porous structure can greatly improve hydrogel is moved back Swelling rate.
And traditional porous aquagel there is also porosity is low, therefore how the not high problem of intensity makes porous aquagel Playing better performance becomes the art one of the technical problems that are urgent to solve.
Summary of the invention
The present invention solves the technical problem of: low for traditional porous aquagel porosity, intensity is not high to be lacked Point provides a kind of preparation method of porous aquagel.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of porous aquagel, specific preparation process is as follows:
(1) according to parts by weight, 40~50 parts of pretreatment acrylamides are successively taken, 8~10 parts of drying oil, 3~5 parts of linoleic acid, 5 ~8 parts of emulsifiers, 8~10 parts of calcium carbonate, 2~3 parts of ammonium persulfates, 10~20 parts of modified additives, 8~10 parts composite foamed Agent, 60~80 parts of water;
(2) acrylamide, drying oil, linoleic acid, emulsifier, calcium carbonate and water mixing will be pre-processed, ammonium persulfate is subsequently added into, The reaction of nitrogen charging heating stirring is subsequently added into modified additive and composite foamable agent, and injection molding is stood, and demoulding obtains blank;
(3) blank is placed in ultrasonic immersing in hydrochloric acid, taken out, it is dry to get porous aquagel.
The preparation process of step (1) described modified additive are as follows: mix polyvinyl alcohol and water 1:30~1:50 in mass ratio It closes, after standing swelling, 0.5~0.8 times of polyvinyl alcohol quality of gelatin is added in heating stirring dissolution, and stirring and dissolving is then added The hydrochloric acid and 8~10 times of polyvinyl alcohol quality of glutaraldehyde solution that 8~10 times of polyvinyl alcohol quality are stirred to react, filtering, stripping and slicing, Washing is dried in vacuo, and is crushed, is obtained modified additive.
Step (1) composite foamable agent be sodium bicarbonate and N, N'- methylene-bisacrylamide 1:1~1 in mass ratio: 2 mixed preparings form.
Step (2) the pretreatment acrylamide is with the acrylamide after acetone recrystallization.
Step (2) the nitrogen charging heating stirring reaction condition are as follows: the rate that is filled with of nitrogen is 100~120mL/min, temperature It is 70~75 DEG C, revolving speed is 300~500r/min.
Step (1) drying oil is linseed oil, any one in tung oil or Chinese catalpa oil.
Step (1) emulsifier is neopelex, alkyl glycosides, any in Tween-80 or Si Pan -80 It is a kind of.
The beneficial effects of the present invention are:
(1) of the invention by adding modified additive and composite foamable agent, it is coagulated in modified gel additive containing sensitive to pH Plastic structure, after being added in product, when near gelatin isoelectric point, gel can be with ring when deviateing isoelectric point in contraction state The change of the pH in border and expand or shrink, in use, firstly, heated point of sodium bicarbonate in composite foamable agent Solution, the gas and sodium carbonate of generation, the gas of generation play foaming effect, so that the porosity of system gets a promotion, secondly, raw At sodium carbonate the pH of system is gradually increasing, carboxylic ions in gelatin are mutually exclusive with negative electrical charge of the same race, modified addition Material expansion, the pressure for expanding generation refine the hole of the generation in system further, again, in heating reaction process In, the gelatin in modified additive is melted by pyrolysis, so that the porosity of system is further promoted;
(2) present invention is by addition drying oil and linoleic acid, in use, due to the aliphatic long-chain structure of drying oil, So that the shock resistance and flexibility of emulsion liquid membrane get a promotion in system, secondly, compared with drying oil, the Asia oil of homogenous quantities Acid can provide more double bonds, and the unsaturated bond increasing proportion in system increases its crosslinking points, further improves product Intensity.
Specific embodiment
Polyvinyl alcohol and water 1:30~1:50 in mass ratio are placed in three-necked flask, stir 10~20min with glass bar, After standing 3~5h of swelling, three-necked flask is placed in digital display and is tested the speed in constant temperature blender with magnetic force, in temperature be 80~85 DEG C, revolving speed Under the conditions of 400~600r/min, heating stirring dissolves 40~60min, and 0.5~0.8 times of polyvinyl alcohol quality of gelatin is added, It is 80~85 DEG C in temperature, under the conditions of revolving speed is 400~600r/min, heating stirring dissolves 40~60min, burns then to three mouthfuls Be added in bottle 8~10 times of polyvinyl alcohol quality of hydrochloric acid and 8~10 times of polyvinyl alcohol quality of glutaraldehyde solution in temperature be 28 ~38 DEG C, revolving speed is stirred 10~12h under conditions of being 250~300r/min, obtains mixed serum, then by mixed serum mistake Filter, obtains gel, by gel stripping and slicing, and is washed with deionized 5~6 days, change a deionized water every 10~12h, will wash Gel piece afterwards obtains desiccant gel block, then desiccant gel block is placed in pulverizer in being dried in vacuo 3~5h under room temperature It crushes, crosses the sieve of 100 mesh, obtain modified additive;According to parts by weight, 40~50 parts of pretreatment acrylamides are successively taken, 8~10 Part drying oil, 3~5 parts of linoleic acid, 5~8 parts of emulsifiers, 8~10 parts of calcium carbonate, 2~3 parts of ammonium persulfates, 10~20 parts of modifications Additive, 8~10 parts of composite foamable agents, 60~80 parts of water;Acrylamide, drying oil, linoleic acid, emulsifier, carbon will be pre-processed Sour calcium and water are added in reaction kettle, and under the conditions of revolving speed is 300~500r/min, ammonium persulfate is then added into reaction kettle, And nitrogen is filled with into kettle with the rate of 100~120mL/min, temperature is 70~75 DEG C, and revolving speed is 300~500r/min condition Under, after nitrogen charging heating stirring reacts 1~2h, modified additive and composite foamable agent, temperature 70 are then added into reaction kettle ~75 DEG C, under the conditions of revolving speed is 300~500r/min, 10~20min of heating stirring obtains mixed slurry, two is sprayed into mold Methyl-silicone oil, then by mixed slurry inject mold in after, stand 18~for 24 hours after, demoulding, obtain blank;Blank is placed in hydrochloric acid In, under the conditions of supersonic frequency is 55~75kHz, after 1~2h of ultrasonic immersing, takes out, the blank after dipping is then placed in baking In case, under the conditions of temperature is 105~110 DEG C, drying is to constant weight to get porous aquagel.The composite foamable agent is carbonic acid Hydrogen sodium and N, N'- methylene-bisacrylamide 1:1~1:2 mixed preparing in mass ratio form.The pretreatment acrylamide is With the acrylamide after acetone recrystallization.The drying oil is linseed oil, any one in tung oil or Chinese catalpa oil.The emulsifier For neopelex, alkyl glycosides, any one in Tween-80 or Si Pan -80.
Example 1
Polyvinyl alcohol and water 1:50 in mass ratio are placed in three-necked flask, stir 20min with glass bar, after standing swelling 5h, Three-necked flask is placed in digital display to test the speed in constant temperature blender with magnetic force, in temperature be 85 DEG C, under the conditions of revolving speed is 600r/min, heating 0.8 times of polyvinyl alcohol quality of gelatin is added in stirring and dissolving 60min, in temperature be 85 DEG C, under the conditions of revolving speed is 600r/min, Heating stirring dissolves 60min, then to hydrochloric acid and the polyvinyl alcohol quality 10 that 10 times of polyvinyl alcohol quality are added in three-necked flask Glutaraldehyde solution again is 38 DEG C in temperature, and revolving speed is stirred 12h under conditions of being 300r/min, obtains mixed serum, then will Mixed serum filtering, obtains gel, by gel stripping and slicing, and is washed with deionized 6 days, change a deionized water every 12h, will wash Gel piece after washing obtains desiccant gel block in being dried in vacuo 5h under room temperature, and then desiccant gel block is placed in pulverizer It crushes, crosses the sieve of 100 mesh, obtain modified additive;According to parts by weight, 50 parts of pretreatment acrylamides, 10 parts of stemness are successively taken Oil, 5 parts of linoleic acid, 8 parts of emulsifiers, 10 parts of calcium carbonate, 3 parts of ammonium persulfates, 20 parts of modified additives, 10 parts of composite foamable agents, 80 parts of water;Acrylamide will be pre-processed, drying oil, linoleic acid, emulsifier, calcium carbonate and water is added in reaction kettle, is in revolving speed Under the conditions of 500r/min, ammonium persulfate is then added into reaction kettle, and nitrogen is filled with into kettle with the rate of 120mL/min, Temperature is 75 DEG C, under the conditions of revolving speed is 500r/min, after nitrogen charging heating stirring reacts 2h, modification is then added into reaction kettle and adds Charging and composite foamable agent, temperature are 75 DEG C, and under the conditions of revolving speed is 500r/min, heating stirring 20min obtains mixed slurry, to Dimethicone is sprayed in mold, after then injecting mixed slurry in mold, after standing for 24 hours, demoulding obtains blank;By blank It is placed in hydrochloric acid, under the conditions of supersonic frequency is 75kHz, after ultrasonic immersing 2h, takes out, the blank after dipping is then placed in baking In case, under the conditions of temperature is 110 DEG C, drying is to constant weight to get porous aquagel.The composite foamable agent be sodium bicarbonate with N, N'- methylene-bisacrylamide 1:2 mixed preparing in mass ratio form.The pretreatment acrylamide is to use acetone recrystallization Acrylamide afterwards.The drying oil is linseed oil.The emulsifier is neopelex.
Example 2
Polyvinyl alcohol and water 1:50 in mass ratio are placed in three-necked flask, stir 20min with glass bar, after standing swelling 5h, Three-necked flask is placed in digital display to test the speed in constant temperature blender with magnetic force, in temperature be 85 DEG C, under the conditions of revolving speed is 600r/min, heating 0.8 times of polyvinyl alcohol quality of gelatin is added in stirring and dissolving 60min, in temperature be 85 DEG C, under the conditions of revolving speed is 600r/min, Heating stirring dissolves 60min, then to hydrochloric acid and the polyvinyl alcohol quality 10 that 10 times of polyvinyl alcohol quality are added in three-necked flask Glutaraldehyde solution again is 38 DEG C in temperature, and revolving speed is stirred 12h under conditions of being 300r/min, obtains mixed serum, then will Mixed serum filtering, obtains gel, by gel stripping and slicing, and is washed with deionized 6 days, change a deionized water every 12h, will wash Gel piece after washing obtains desiccant gel block in being dried in vacuo 5h under room temperature, and then desiccant gel block is placed in pulverizer It crushes, crosses the sieve of 100 mesh, obtain modified additive;According to parts by weight, 50 parts of pretreatment acrylamides, 5 parts of sub- oil are successively taken Acid, 8 parts of emulsifiers, 10 parts of calcium carbonate, 3 parts of ammonium persulfates, 20 parts of modified additives, 10 parts of composite foamable agents, 80 parts of water;It will be pre- Processing acrylamide, linoleic acid, emulsifier, calcium carbonate and water are added in reaction kettle, under the conditions of revolving speed is 500r/min, then Ammonium persulfate is added into reaction kettle, and nitrogen is filled with into kettle with the rate of 120mL/min, temperature is 75 DEG C, and revolving speed is Under the conditions of 500r/min, after nitrogen charging heating stirring reacts 2h, modified additive and composite foamable agent are then added into reaction kettle, Temperature is 75 DEG C, and under the conditions of revolving speed is 500r/min, heating stirring 20min obtains mixed slurry, dimethyl-silicon is sprayed into mold Oil, after then injecting mixed slurry in mold, after standing for 24 hours, demoulding obtains blank;Blank is placed in hydrochloric acid, in supersonic frequency Rate be 75kHz under the conditions of, after ultrasonic immersing 2h, take out, then the blank after dipping is placed in baking oven, in temperature be 110 DEG C Under the conditions of, drying is to constant weight to get porous aquagel.The composite foamable agent is sodium bicarbonate and N, N'- methylene bisacrylamide Amide 1:2 mixed preparing in mass ratio forms.The pretreatment acrylamide is with the acrylamide after acetone recrystallization.It is described Emulsifier is neopelex.
Example 3
Polyvinyl alcohol and water 1:50 in mass ratio are placed in three-necked flask, stir 20min with glass bar, after standing swelling 5h, Three-necked flask is placed in digital display to test the speed in constant temperature blender with magnetic force, in temperature be 85 DEG C, under the conditions of revolving speed is 600r/min, heating 0.8 times of polyvinyl alcohol quality of gelatin is added in stirring and dissolving 60min, in temperature be 85 DEG C, under the conditions of revolving speed is 600r/min, Heating stirring dissolves 60min, then to hydrochloric acid and the polyvinyl alcohol quality 10 that 10 times of polyvinyl alcohol quality are added in three-necked flask Glutaraldehyde solution again is 38 DEG C in temperature, and revolving speed is stirred 12h under conditions of being 300r/min, obtains mixed serum, then will Mixed serum filtering, obtains gel, by gel stripping and slicing, and is washed with deionized 6 days, change a deionized water every 12h, will wash Gel piece after washing obtains desiccant gel block in being dried in vacuo 5h under room temperature, and then desiccant gel block is placed in pulverizer It crushes, crosses the sieve of 100 mesh, obtain modified additive;According to parts by weight, 50 parts of pretreatment acrylamides, 10 parts of stemness are successively taken Oil, 8 parts of emulsifiers, 10 parts of calcium carbonate, 3 parts of ammonium persulfates, 20 parts of modified additives, 10 parts of composite foamable agents, 80 parts of water;It will be pre- Processing acrylamide, drying oil, emulsifier, calcium carbonate and water are added in reaction kettle, under the conditions of revolving speed is 500r/min, then Ammonium persulfate is added into reaction kettle, and nitrogen is filled with into kettle with the rate of 120mL/min, temperature is 75 DEG C, and revolving speed is Under the conditions of 500r/min, after nitrogen charging heating stirring reacts 2h, modified additive and composite foamable agent are then added into reaction kettle, Temperature is 75 DEG C, and under the conditions of revolving speed is 500r/min, heating stirring 20min obtains mixed slurry, dimethyl-silicon is sprayed into mold Oil, after then injecting mixed slurry in mold, after standing for 24 hours, demoulding obtains blank;Blank is placed in hydrochloric acid, in supersonic frequency Rate be 75kHz under the conditions of, after ultrasonic immersing 2h, take out, then the blank after dipping is placed in baking oven, in temperature be 110 DEG C Under the conditions of, drying is to constant weight to get porous aquagel.The composite foamable agent is sodium bicarbonate and N, N'- methylene bisacrylamide Amide 1:2 mixed preparing in mass ratio forms.The pretreatment acrylamide is with the acrylamide after acetone recrystallization.It is described Drying oil is linseed oil.The emulsifier is neopelex.
Example 4
According to parts by weight, 50 parts of pretreatment acrylamides are successively taken, 10 parts of drying oil, 5 parts of linoleic acid, 8 parts of emulsifiers, 10 parts Calcium carbonate, 3 parts of ammonium persulfates, 10 parts of composite foamable agents, 80 parts of water;Acrylamide, drying oil, linoleic acid, emulsification will be pre-processed Agent, calcium carbonate and water are added in reaction kettle, and under the conditions of revolving speed is 500r/min, ammonium persulfate is then added into reaction kettle, And nitrogen is filled with into kettle with the rate of 120mL/min, temperature is 75 DEG C, and under the conditions of revolving speed is 500r/min, nitrogen charging heating is stirred After mixing reaction 2h, composite foamable agent is then added into reaction kettle, temperature is 75 DEG C, under the conditions of revolving speed is 500r/min, heating 20min is stirred, mixed slurry is obtained, dimethicone is sprayed into mold, after then injecting mixed slurry in mold, is stood After for 24 hours, demoulding obtains blank;Blank is placed in hydrochloric acid, under the conditions of supersonic frequency is 75kHz, after ultrasonic immersing 2h, is taken out, Then the blank after dipping is placed in baking oven, under the conditions of temperature is 110 DEG C, drying is to constant weight to get porous aquagel.Institute Stating composite foamable agent is sodium bicarbonate and N, and N'- methylene-bisacrylamide 1:2 mixed preparing in mass ratio forms.The pre- place Managing acrylamide is with the acrylamide after acetone recrystallization.The drying oil is linseed oil.The emulsifier is dodecyl Benzene sulfonic acid sodium salt.
Example 5
Polyvinyl alcohol and water 1:50 in mass ratio are placed in three-necked flask, stir 20min with glass bar, after standing swelling 5h, Three-necked flask is placed in digital display to test the speed in constant temperature blender with magnetic force, in temperature be 85 DEG C, under the conditions of revolving speed is 600r/min, heating 0.8 times of polyvinyl alcohol quality of gelatin is added in stirring and dissolving 60min, in temperature be 85 DEG C, under the conditions of revolving speed is 600r/min, Heating stirring dissolves 60min, then to hydrochloric acid and the polyvinyl alcohol quality 10 that 10 times of polyvinyl alcohol quality are added in three-necked flask Glutaraldehyde solution again is 38 DEG C in temperature, and revolving speed is stirred 12h under conditions of being 300r/min, obtains mixed serum, then will Mixed serum filtering, obtains gel, by gel stripping and slicing, and is washed with deionized 6 days, change a deionized water every 12h, will wash Gel piece after washing obtains desiccant gel block in being dried in vacuo 5h under room temperature, and then desiccant gel block is placed in pulverizer It crushes, crosses the sieve of 100 mesh, obtain modified additive;According to parts by weight, 50 parts of pretreatment acrylamides, 10 parts of stemness are successively taken Oil, 5 parts of linoleic acid, 8 parts of emulsifiers, 10 parts of calcium carbonate, 3 parts of ammonium persulfates, 20 parts of modified additives, 80 parts of water;It will pretreatment Acrylamide, drying oil, linoleic acid, emulsifier, calcium carbonate and water are added in reaction kettle, under the conditions of revolving speed is 500r/min, Then ammonium persulfate is added into reaction kettle, and nitrogen is filled with into kettle with the rate of 120mL/min, temperature is 75 DEG C, revolving speed Under the conditions of 500r/min, after nitrogen charging heating stirring reacts 2h, modified additive, temperature 75 are then added into reaction kettle DEG C, under the conditions of revolving speed is 500r/min, heating stirring 20min obtains mixed slurry, dimethicone is sprayed into mold, then After mixed slurry is injected in mold, after standing for 24 hours, demoulding obtains blank;Blank is placed in hydrochloric acid, is in supersonic frequency Under the conditions of 75kHz, after ultrasonic immersing 2h, take out, then the blank after dipping is placed in baking oven, in temperature be 110 DEG C of conditions Under, drying is to constant weight to get porous aquagel.The pretreatment acrylamide is with the acrylamide after acetone recrystallization.Institute Stating drying oil is linseed oil.The emulsifier is neopelex.
Comparative example: the porous aquagel of Foshan Science and Technology Ltd. production.
Example 1 to the resulting porous aquagel of example 5 and comparative example product are subjected to performance detection, specific detection method is such as Under:
By test specimen according to GB/T1040 Erichsen test method sample preparation, its tensile strength is measured with universal testing machine and fracture is stretched Long rate, rate of extension 500mm/min measure 20 DEG C of temperature, measure humidity 70%;And use mercury injection apparatus (Autopore9500) Measurement detection test specimen porosity.
Specific testing result is as shown in table 1:
The specific testing result of 1 porous aquagel of table
By 1 testing result of table it is found that the porous aquagel of technical solution of the present invention preparation has the characteristics that porosity and intensity are high, It has broad prospects in the development of high polymer material technology industry.

Claims (7)

1. a kind of preparation method of porous aquagel, it is characterised in that specific preparation process is as follows:
(1) according to parts by weight, 40~50 parts of pretreatment acrylamides are successively taken, 8~10 parts of drying oil, 3~5 parts of linoleic acid, 5 ~8 parts of emulsifiers, 8~10 parts of calcium carbonate, 2~3 parts of ammonium persulfates, 10~20 parts of modified additives, 8~10 parts composite foamed Agent, 60~80 parts of water;
(2) acrylamide, drying oil, linoleic acid, emulsifier, calcium carbonate and water mixing will be pre-processed, ammonium persulfate is subsequently added into, The reaction of nitrogen charging heating stirring is subsequently added into modified additive and composite foamable agent, and injection molding is stood, and demoulding obtains blank;
(3) blank is placed in ultrasonic immersing in hydrochloric acid, taken out, it is dry to get porous aquagel.
2. a kind of preparation method of porous aquagel according to claim 1, it is characterised in that: step (1) described modification adds Add the preparation process of agent are as follows: mix polyvinyl alcohol with water 1:30~1:50 in mass ratio, after standing swelling, heating stirring is molten Solution, is added 0.5~0.8 times of polyvinyl alcohol quality of gelatin, and 8~10 times of polyvinyl alcohol quality of salt is then added in stirring and dissolving Acid and 8~10 times of polyvinyl alcohol quality of glutaraldehyde solution are stirred to react, and are filtered, stripping and slicing, are washed, and are dried in vacuo, and are crushed, must be changed Property additive.
3. a kind of preparation method of porous aquagel according to claim 1, it is characterised in that: step (1) the compound hair Infusion is sodium bicarbonate and N, and N'- methylene-bisacrylamide 1:1~1:2 mixed preparing in mass ratio forms.
4. a kind of preparation method of porous aquagel according to claim 1, it is characterised in that: step (2) described pretreatment Acrylamide is with the acrylamide after acetone recrystallization.
5. a kind of preparation method of porous aquagel according to claim 1, it is characterised in that: step (2) described nitrogen charging adds Thermal agitation reaction condition are as follows: nitrogen be filled with rate be 100~120mL/min, temperature be 70~75 DEG C, revolving speed be 300~ 500r/min。
6. a kind of preparation method of porous aquagel according to claim 1, it is characterised in that: step (1) described drying oil For linseed oil, tung oil or Chinese catalpa oil in any one.
7. a kind of preparation method of porous aquagel according to claim 1, it is characterised in that: step (1) described emulsifier For neopelex, alkyl glycosides, any one in Tween-80 or Si Pan -80.
CN201810727061.6A 2018-07-05 2018-07-05 A kind of preparation method of porous aquagel Withdrawn CN109232958A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810727061.6A CN109232958A (en) 2018-07-05 2018-07-05 A kind of preparation method of porous aquagel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810727061.6A CN109232958A (en) 2018-07-05 2018-07-05 A kind of preparation method of porous aquagel

Publications (1)

Publication Number Publication Date
CN109232958A true CN109232958A (en) 2019-01-18

Family

ID=65071723

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810727061.6A Withdrawn CN109232958A (en) 2018-07-05 2018-07-05 A kind of preparation method of porous aquagel

Country Status (1)

Country Link
CN (1) CN109232958A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109943083A (en) * 2019-02-20 2019-06-28 庄文琴 A kind of preparation method of stretch-proof compound rubber asphalt mixture

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1683441A (en) * 2005-03-11 2005-10-19 清华大学 Process for preparing biologically degradable reverse temperature sensitive material
US20080032092A1 (en) * 2000-08-07 2008-02-07 Tennison Stephen R Porous carbons
CN102633956A (en) * 2012-04-27 2012-08-15 海洋化工研究院 Preparation method of porous hydrogel and application thereof
CN104356319A (en) * 2014-11-03 2015-02-18 四川大学 Porous biological material using modified gelatin as crosslinking agent and preparation method of porous biological material
CN105161315A (en) * 2015-09-16 2015-12-16 中国科学院电工研究所 Hydrogel electrolyte thin film, and preparation method and application therefor

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080032092A1 (en) * 2000-08-07 2008-02-07 Tennison Stephen R Porous carbons
CN1683441A (en) * 2005-03-11 2005-10-19 清华大学 Process for preparing biologically degradable reverse temperature sensitive material
CN102633956A (en) * 2012-04-27 2012-08-15 海洋化工研究院 Preparation method of porous hydrogel and application thereof
CN104356319A (en) * 2014-11-03 2015-02-18 四川大学 Porous biological material using modified gelatin as crosslinking agent and preparation method of porous biological material
CN105161315A (en) * 2015-09-16 2015-12-16 中国科学院电工研究所 Hydrogel electrolyte thin film, and preparation method and application therefor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109943083A (en) * 2019-02-20 2019-06-28 庄文琴 A kind of preparation method of stretch-proof compound rubber asphalt mixture

Similar Documents

Publication Publication Date Title
CN103923428A (en) Starch-based porous hydrogel and preparation method thereof
CN103804700B (en) A kind of preparation method of photonic crystal hydrogel of chemically crosslinked of Color tunable
CN111057251B (en) Preparation method of cationic hydrogel
CN106810704B (en) Polyvinyl alcohol hydrogel and its preparation method and application
CN104845382A (en) Silk protein/cellulose derivative blending hydrogel and preparation method thereof
CN104307389B (en) Polyether sulfone thermal stimulus response film and preparation method thereof
CN110483813A (en) A kind of preparation method of room temperature photo-thermal selfreparing hydrogel
CN110078945A (en) A kind of preparation method of gelatin-based high intensity hydrogel
CN109503768A (en) A kind of preparation method of high tough sticky weather-resistance polyethylene alcohol radical double-network hydrogel
CN110407980A (en) A kind of preparation method of cellulosic polymer surfactant base pH and the double response type composite hydrogels of temperature
CN109232958A (en) A kind of preparation method of porous aquagel
MORITAKA et al. Rheological properties of aqueous agarose‐gelatin gels
Ju et al. Effects of internal microstructures of poly (N-isopropylacrylamide) hydrogels on thermo-responsive volume phase-transition and controlled-release characteristics
CN105001442A (en) Method for preparing porous hydrogel through micropore self foaming
CN105778123A (en) Agar and graphene oxide double-network hydrogel and preparation method thereof
CN110452480B (en) Preparation method of ultra-light heat-insulating flexible aerogel
CN104861218B (en) Chitin potassium titanate composite crystal palpus film and preparation method thereof
CN109181014A (en) A kind of preparation method of the aqueous core model material of high-strength stable
CN1935271A (en) Method for preparing chitosan or/and gelatin-polylacticacid polymer blend three-dimensional porous stent
CN109180879A (en) A kind of preparation method of leak stopping oil well cement paste thixotropic agent
CN109382002A (en) A kind of intelligent switch film and preparation method thereof based on nanogel
WO2019047043A1 (en) Silk fibroin/chitosan composite smart hydrogel and preparation method therefor
CN110623250B (en) Preparation method of cellulose nanocrystal-whey protein isolate composite thermal gel
CN104998298A (en) Chitosan support achieving directional hole forming and preparation method of chitosan support
CN109749306A (en) A kind of perforated foams and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication
WW01 Invention patent application withdrawn after publication

Application publication date: 20190118