CN108159023A - A kind of preparation method and product of cold compress hydrogel plaster - Google Patents
A kind of preparation method and product of cold compress hydrogel plaster Download PDFInfo
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- CN108159023A CN108159023A CN201711400373.8A CN201711400373A CN108159023A CN 108159023 A CN108159023 A CN 108159023A CN 201711400373 A CN201711400373 A CN 201711400373A CN 108159023 A CN108159023 A CN 108159023A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/70—Web, sheet or filament bases ; Films; Fibres of the matrix type containing drug
- A61K9/7023—Transdermal patches and similar drug-containing composite devices, e.g. cataplasms
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F7/00—Heating or cooling appliances for medical or therapeutic treatment of the human body
- A61F7/02—Compresses or poultices for effecting heating or cooling
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
- A61K47/10—Alcohols; Phenols; Salts thereof, e.g. glycerol; Polyethylene glycols [PEG]; Poloxamers; PEG/POE alkyl ethers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/34—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyesters, polyamino acids, polysiloxanes, polyphosphazines, copolymers of polyalkylene glycol or poloxamers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0208—Tissues; Wipes; Patches
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0212—Face masks
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/85—Polyesters
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/86—Polyethers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/005—Preparations for sensitive skin
-
- 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
- C08F261/00—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
- C08F261/02—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols
- C08F261/04—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols on to polymers of vinyl alcohol
-
- 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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- 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
- C08F8/00—Chemical modification by after-treatment
- C08F8/14—Esterification
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
- C08G65/3322—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof acyclic
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F7/00—Heating or cooling appliances for medical or therapeutic treatment of the human body
- A61F7/02—Compresses or poultices for effecting heating or cooling
- A61F2007/0203—Cataplasms, poultices or compresses, characterised by their contents; Bags therefor
Abstract
The invention discloses a kind of cold compress hydrogel plaster and preparation method thereof, including：(1) in the presence of esterification catalyst, polyethylene glycol, polyvinyl alcohol and acrylic acid carry out esterification, obtain polyethylene glycol, polyvinyl alcohol acrylic acid mixed ester；(2) polyethylene glycol, polyvinyl alcohol acrylic acid mixed ester and aqueous tackifier resin, crosslinking agent, photoinitiator, moisturizer, mould inhibitor, cooling agent, water are mixed to get cold compress water-setting collagen solution；(3) obtained cold compress with water-setting collagen solution on coating machine is continuously coated on base material, and through ultraviolet lighting curing gel, it is cut, is packed up to hydrogel plaster product.The production technology raw material sources that hydrogel plaster is prepared using this method are convenient, and manufacture craft is simple, and gel solidification is rapid, complete, it is suitble to volume production, the series of advantages such as products obtained therefrom has stable storing, and bubble-free, transparency are high, cooling-down effect is apparent, and applicating property and moisture retention are good.
Description
Technical field
The invention belongs to therapeutic physical education articles for use hydrogel plaster production fields, are specifically related to a kind of cold compress hydrogel plaster
Preparation method.
Background technology
Hydrogel plaster, also known as modern cataplasm, mainly by hydrophilic resin, crosslinking agent, moisturizer, pure water, function
Property additive and water-swellable cross-linked polymer etc. is into being grouped as.It is mainly used for external-use gel patch, optimum wound location
Cold compress, be applied with.
For traditional cataplasm earliest originating from Japan, initially kaolinite bar cloth, production method is usually by paddy such as oatmeals
Object and water, breast, wax etc. mix, then mix drug and purees is made, and are fitted into closed container, and when use is coated on gauze, paste
In affected part, referred to as pureed cataplasm (poultice).This preparation stickiness is insufficient, and cohesion force difference, pollution clothes are inconvenient for use, class
Like the cataplasm of tcm in China.It is in nineteen seventies, with Japanese pharmaceutical industrial chemicals that cataplasm, which is really developed,
The extensive use of industrial expansion and high molecular material selects provide convenience condition, particularly polypropylene for catablasm base material
The use of sour sodium, makes it make a breakthrough on matrix formulations, is had evolved into so far using hydrophilic high molecular polymer as master
Want molding cataplasm --- the hydrogel plaster of matrix scaffold.
Modern hydrogel patch construction is mainly made of back sheet, hydrogel matrix layer and protection or adherent layer three parts,
It is wherein mostly important with hydrogel matrix layer.
Hydrogel generally by with three-dimensional network stereochemical structure high molecular material prepare, in water do not dissolve but can be molten
It is swollen, and certain mechanical property and very high water content can be kept, compliance and biocompatibility are good, so as to make hydrogel
Patch has the particular advantages better than traditional cataplasm, and such as drugloading rate height, dosage is accurate, and applicating property and moisture retention are good, no sensitization
Property and irritation, easy to use, comfortable, pollution clothes, will not occur the adverse reactions such as lead poisoning.
Especially as the hydrogel plaster of cold compress, because rich in moisture, having to surface of a wound moisturizing and absorbing the dual of sepage
Effect, can keep the surface of a wound to moisten, can effectively avoid the dry necrosis of wound tissue, play exogenous debridement effect, can improve wound
The power of regeneration of mouth granulation tissue, and accelerate wound healing, and be not easy to stay scar, feature energy that is comfortable, soft, being rich in elasticity
Mitigate wound pain；The adhesion surface of a wound when removing dressing, avoids the secondary damage of the surface of a wound, and hydrogel plaster is oozed in absorption wound
It is not loose after liquid, do not crush, noresidue, high transparency can directly observe wound and its variation.Therefore, modern hydrogel
Patch is a kind of novel patch of great use value.
But the preparation process of existing hydrogel plaster, framework material add crosslinking agent by water soluble polymer mostly
Be cross-linked to form (such as Publication No. CN 102614517A patent documents), since cross-linking reaction speed is difficult to control, skeleton material
The agent structure of material quickly forms within a short period of time, causes that system viscosity is quick, significantly rises, to the coating of hydrogel plaster
Glue-applying technique brings extreme difficulties, and product is caused a systems such as be unevenly coated, the dispersion of more bubbles, functional additive is not easy occur
Column defects, and the fully crosslinked reaction of hydrogel backbone material is also difficult to be completed in a short time, and sticker is cut too early
It cuts, pack the broken of hydrogel, adhesion can be caused to occur, it is very difficult so as to cause the volume production of product.
Invention content
To overcome the existing drawbacks described above for preparing hydrogel plaster, the present invention provides a kind of preparations of cold compress hydrogel plaster
Method.The production technology raw material sources that hydrogel plaster is prepared using this method are convenient, and manufacture craft is simple, and crosslinking rate is controllable,
Gel solidification is rapid, complete, is suitble to volume production.
The present invention also provides a kind of hydrogel plaster product, which has stable storing, and bubble-free, transparency are high, drop
The series of advantages such as temp effect is apparent, and applicating property and moisture retention are good.
The present invention provides a kind of preparation methods of cold compress hydrogel plaster, include the following steps：
(1) in the presence of esterification catalyst, polyethylene glycol, polyvinyl alcohol and acrylic acid carry out esterification, obtain poly- second
Glycol, polyvinyl alcohol-acrylic acid mixed ester；
(2) polyethylene glycol, polyvinyl alcohol-acrylic acid mixed ester and the aqueous tackifier resin that obtain step (1) are handed over
Connection agent, photoinitiator, moisturizer, mould inhibitor, cooling agent, water are mixed to get cold compress water-setting collagen solution；The crosslinking agent is third
Olefin(e) acid ester crosslinking agent；
(3) cold compress that step (2) obtains continuously is coated on base material, and on coating machine through ultraviolet with water-setting collagen solution
Illumination curing gel is cut it, is packed up to hydrogel plaster product.
Further, the present invention provides cold compress hydrogel plaster preparation method, include the following steps：
(1) preparation of hydrogel backbone material --- polyethylene glycol, polyvinyl alcohol-acrylic acid mixed ester：
First, raw material polyethylene glycol, polyvinyl alcohol are opened as in reaction kettle of the metering input with water knockout drum and condenser
Dynamic blender is heated to 90~95 DEG C, and insulated and stirred is complete to polyvinyl alcohol dissolving；Then 50~60 DEG C are cooled to, by metering
Add in acrylic acid, water entrainer, polymerization inhibitor, catalyst, be heated to reaction system and backflow phenomenon occur, and maintain at this temperature into
Row reaction；Stop heating when reaction is largely distilled out of to theoretical water yield, reaction was completed, then is cooled to 40 DEG C hereinafter, mistake
Solid catalyst is filtered out, vacuum extracts and recycling design, and it is spare to obtain polyethylene glycol, polyvinyl alcohol-acrylic acid mixed ester.
(2) preparation of cold compress water-setting collagen solution
Polyethylene glycol, polyvinyl alcohol-acrylic acid mixed ester and aqueous tackifier resin that step (1) is obtained, crosslinking
Agent, photoinitiator, moisturizer, mould inhibitor, cooling agent, pure water etc. are uniformly mixed, and are proportionally added into mixing kettle, are stirred at room temperature
30~60min, then 10~20min of vacuumizing and defoaming, discharging are spare.
(3) preparation of cold compress hydrogel plaster
The cold compress that step (2) obtains continuously is coated on base material, and on coating machine through ultraviolet light with water-setting collagen solution
According to curing gel, it is cut, is packed up to hydrogel plaster product.
In preferred technical solution, calculate in percentage by weight, raw material includes in the step (1)：
Raw material includes in the step (2)：
In above-mentioned raw materials, the molecular weight of the polyethylene glycol is 400~600.
Preferably, the water entrainer includes one or more of benzene,toluene,xylene mixture.It selects
Above-mentioned water entrainer while reaction dissolvent is served as, ensures that the moisture of generation is detached from system in time, promotes esterification thorough rapidly
The progress at bottom, avoids additional operation.
Preferably, the catalyst is the dedicated solid acid catalyst of esterification.It can be used common in the market
Esterification solid acid catalyst.For example, can be used the big synthesis Chemical Co., Ltd. in Jiangyin City south HND series of products (including
HND-31 solid super acid catalysts, HND-32 solid super acid catalysts, HND-33 solid super acid catalysts, HND-34 are solid
Body super acidic catalyst etc.).Solid acid catalyst is selected, reduces waste liquor contamination, while convenient for the recycling of catalyst, reduce
Production cost.
Preferably, the polymerization inhibitor includes one kind in hydroquinone, tert-butyl catechol, p-hydroxyanisole
Or two or more mixtures.
Preferably, the aqueous tackifier resin includes polyvinylpyrrolidone, sodium carboxymethylcellulose, ethoxy fibre
Tie up one or more of element mixture.Cold compress water-setting of the present invention can be adjusted by adjusting the amount of aqueous tackifier resin
The viscosity of collagen solution, so as to quick, efficient, high quality the completion of follow-up painting work.
Preferably, the crosslinking agent includes glycol diacrylate, trimethylolpropane trimethacrylate, season penta
One or more of tetrol triacrylate mixture.
Preferably, the photoinitiator includes one in benzoin methyl ether, benzoin ethyl ether, dihydroxy benaophenonel
Kind or two or more mixtures.
The present invention is used cooperatively using polyethylene glycol, polyvinyl alcohol-acrylic acid mixed ester with above-mentioned acrylate cross linked dose,
It is combined above-mentioned photoinitiator simultaneously；By adjusting polyethylene glycol, polyvinyl alcohol-acrylic acid mixed ester and crosslinking agent and photoinitiator
Proportioning, while pass through the control to photocuring parameter so that：On the one hand, before ultraviolet lighting, it ensure that cold compress hydrogel
Stoste has relatively low viscosity, convenient for painting work；Meanwhile in coating process, pass through the control of Light Curing technological parameter
System ensure that crosslinking curing speed, ensures that coating is more uniform, reduces the generation of bubble；Moreover, also ensure crosslinking curing
Rapid progress, while ensureing product quality, save the time so that it is a large amount of that preparation method of the invention is more suitable for industrialization
The technical issues of production, solves in the prior art, and hardening time is long, and product quality is bad.
Preferably, the moisturizer includes one or more of polyalcohols such as glycerine, propylene glycol, butanediol
Mixture.
Preferably, the mould inhibitor include sodium benzoate, potassium sorbate, one kind in parabens mould inhibitor or
Two or more mixtures.
Preferably, the cooling agent include one or both of absolute ethyl alcohol, medicinal alcohol, Peppermint essential oil etc. with
Upper mixture.
Preferably, the ultraviolet lighting wavelength is 365~395nm；The ultraviolet lighting time is 15s~10min, can basis
Actual needs control.Common ultraviolet lamp can be used to be irradiated, can also be shone using highly efficient LED ultraviolet lamps
It penetrates.
First mixed ester is made certainly in polyethylene glycol, polyvinyl alcohol and acrylic acid by the present invention, then using mixed ester as skeleton
Material adds in photoinitiator, crosslinking agent, moisturizer, mould inhibitor, cooling agent, aqueous tackifier resin, pure water etc. and is uniformly mixed,
Cold compress hydrogel plaster is can be made into using ultraviolet lighting curing gel.The cold compress hydrogel plaster being prepared, it is main to use
In external-use gel patch, such as pulled muscle, galling, swelling and pain, wound caused by sprain for exercise, unexpected tumble injury, shock, fracture etc.
Cold compress, external application of situations such as bleeding etc., it can also be used to hydrogel infantile umbilical paste, hydrogel eye paste, hydrogel eye pocket facing, water
Gel mask patch etc..
The invention has the advantages that：
1. polyethylene glycol, polyvinyl alcohol, acrylic acid is selected, which directly to carry out esterification synthesis mixed ester conduct, prepares water-setting
The framework material of glue has the characteristics that raw material is easy to get, synthesis technology is simple, advantage of lower cost, and the transparency of made product is high,
The degree of cross linking is controllable, and the scope of application is wider.
2. by polyethylene glycol, polyvinyl alcohol-acrylic acid mixed ester and photoinitiator, moisturizer, mould inhibitor, cooling agent, water
Property tackifying resin, pure water when preparing water-setting collagen solution, system initial viscosity is little, is conducive to the homodisperse of material, body
System's row's bubble is convenient, and the painting work preferably on hydrogel substrate；
3. cause the gelation cross-linking reaction of polyethylene glycol, polyvinyl alcohol-acrylic acid mixed ester by ultraviolet lighting, and most
For end form into hydrogel backbone, gel forming process control, gel solidification is rapid, and the reaction was complete, and production efficiency significantly rises, and fits
Close the volume production of product.
In conclusion the production technology raw material sources that hydrogel plaster is prepared using this method are convenient, manufacture craft is simple, coagulates
Adhesive curing is rapid, complete, is suitble to volume production, and products obtained therefrom has stable storing, and bubble-free, transparency are high, cooling-down effect is apparent, patch
The series of advantages such as deposited property and moisture retention are good.
Specific embodiment
Embodiment 1
First, in the reaction kettle with condenser and water knockout drum, 300.00kg Macrogol 600s, 200.00kg are added in
Polyethylene glycol 400 starts blender, adds 25.00kg polyvinyl alcohol, is heated to 95 DEG C, insulated and stirred is molten to polyvinyl alcohol
Solution is complete；60 DEG C are then cooled to, adds in 80.10kg acrylic acid, 259.00g hydroquinones, 260.00kg dimethylbenzene, 0.87kg
Solid acid catalyst (the HND-31 solid super acid catalysts purchased from the big synthesis Chemical Co., Ltd. in Jiangyin City south), is heated to anti-
System is answered backflow phenomenon occur, and maintains to be reacted at this temperature；It (is steamed when reaction to theoretical water yield is largely distilled out of
Water outlet is divided into more than the 90% of theoretical moisture) when, stop heating, reaction was completed, is cooled to 40.0 DEG C, discharging filters out recycling solid
Acid catalyst, then vacuum is sent into closed stirred tank to extract simultaneously recycling design dimethylbenzene, it discharges up to polyethylene glycol, polyethylene
Alcohol-acrylic acid mixed ester is spare.
Then, the preparation of cold compress water-setting collagen solution is carried out：
By the polyethylene glycol of above-mentioned preparation, polyvinyl alcohol-acrylic acid mixed ester 60.00kg, polyvinylpyrrolidone
5.00kg, trimethylolpropane trimethacrylate 1.00kg, benzoin methyl ether 1.00kg, glycerine 180.00kg, ethylparaben
3.00kg, absolute ethyl alcohol 50.00kg, pure water 700.00kg etc. are added in mixing kettle, start blender, 30min is stirred at room temperature,
Then vacuumizing and defoaming 10min, discharging are spare.
The cold compress of above-mentioned preparation is continuously coated on base material, and consolidate through ultraviolet lighting with water-setting collagen solution on coating machine
Change gel (365nm ultraviolet lamps irradiate 30s), it is cut, is packed up to hydrogel plaster product.
It is observed that test, hydrogel plaster transparency is good, bubble-free, sticks on that skin surface is not broken, does not stay glue, skin without
Allergic reaction, stick~20min skin surface temperatures can reduce~6 DEG C.
Embodiment 2
First, in the reaction kettle with condenser and water knockout drum, 300.00kg Macrogol 600s, 200.00kg are added in
Polyethylene glycol 400 starts blender, adds 15.00kg polyvinyl alcohol, is heated to 90 DEG C, insulated and stirred is molten to polyvinyl alcohol
Solution is complete；Then be cooled to 50 DEG C, add in 82.00kg acrylic acid, 80.00g tert-butyl catechols, 200.00kg benzene,
2.40kg solid acid catalysts (purchased from the big synthesis Chemical Co., Ltd. HND-33 solid super acid catalysts in Jiangyin City south), heating
There is backflow phenomenon to reaction system, and maintain to be reacted at this temperature；When reaction to theoretical water yield is largely steamed
When going out, stop heating, reaction was completed, is cooled to 40.0 DEG C, discharging filters out recycling solid acid catalyst, then send to closed stirred tank
Middle vacuum extracts and recycling design benzene, discharges spare up to polyethylene glycol, polyvinyl alcohol-acrylic acid mixed ester.
Then, the preparation of cold compress water-setting collagen solution is carried out：
By the polyethylene glycol of above-mentioned preparation, polyvinyl alcohol-acrylic acid mixed ester 40.00kg, polyvinylpyrrolidone
15.00kg, sodium carboxymethylcellulose 10.00kg, pentaerythritol triacrylate 5.00kg, benzoin ethyl ether 0.50kg, glycerine
100.00kg, propylene glycol 100.00kg, sodium benzoate 1.00kg, absolute ethyl alcohol 90.00kg, Peppermint essential oil 10.00kg, pure water
628.50kg etc. is added in mixing kettle, is started blender, 45min is stirred at room temperature, then vacuumizing and defoaming 15min, and discharging is spare.
The cold compress of above-mentioned preparation is continuously coated on base material, and consolidate through ultraviolet lighting with water-setting collagen solution on coating machine
Change gel (365nm ultraviolet lamps irradiate 30s), it is cut, is packed up to hydrogel plaster product.
It is observed that test, hydrogel plaster transparency is good, bubble-free, sticks on that skin surface is not broken, does not stay glue, skin without
Allergic reaction, stick~20min skin surface temperatures can reduce~10 DEG C.
Embodiment 3
First, in the reaction kettle with condenser and water knockout drum, 300.00kg Macrogol 600s, 200.00kg are added in
Polyethylene glycol 400 starts blender, adds 20.00kg polyvinyl alcohol, is heated to 93 DEG C, insulated and stirred is molten to polyvinyl alcohol
Solution is complete；Then be cooled to 55 DEG C, add in 81.30kg acrylic acid, 167.00g p-hydroxyanisole, 233.00kg toluene,
1.25kg solid acid catalysts (purchased from the big synthesis Chemical Co., Ltd. HND-34 solid super acid catalysts in Jiangyin City south), heating
There is backflow phenomenon to reaction system, and maintain to be reacted at this temperature；When reaction to theoretical water yield is largely steamed
When going out, stop heating, reaction was completed, is cooled to 40.0 DEG C, discharging filters out recycling solid acid catalyst, then send to closed stirred tank
Middle vacuum extracts and recycling design toluene, discharges spare up to polyethylene glycol, polyvinyl alcohol-acrylic acid mixed ester.
Then, the preparation of cold compress water-setting collagen solution is carried out：
By the polyethylene glycol of above-mentioned preparation, polyvinyl alcohol-acrylic acid mixed ester 50.00kg, polyvinylpyrrolidone
10.00kg, hydroxyethyl cellulose 5.00kg, glycol diacrylate 3.00kg, dihydroxy benaophenonel 0.80kg, glycerine
100.00kg, propylene glycol 50.00kg, potassium sorbate 1.00kg, butyl hydroxybenzoate 1.00kg, medicinal alcohol 80.00kg, pure water
699.20kg etc. is added in mixing kettle, is started blender, 60min is stirred at room temperature, then vacuumizing and defoaming 20min, and discharging is spare.
The cold compress of above-mentioned preparation is continuously coated on base material, and consolidate through ultraviolet lighting with water-setting collagen solution on coating machine
Change gel (365nmLED lamps irradiate 15s), it is cut, is packed up to hydrogel plaster product.
It is observed that test, hydrogel plaster transparency is good, bubble-free, sticks on that skin surface is not broken, does not stay glue, skin without
Allergic reaction, stick~20min skin surface temperatures can reduce~8 DEG C.
Claims (10)
1. a kind of preparation method of cold compress hydrogel plaster, which is characterized in that include the following steps：
(1) in the presence of esterification catalyst, polyethylene glycol, polyvinyl alcohol and acrylic acid carry out esterification, obtain polyethylene glycol,
Polyvinyl alcohol-acrylic acid mixed ester；
(2) polyethylene glycol, polyvinyl alcohol-acrylic acid mixed ester and the aqueous tackifier resin that obtain step (1), crosslinking agent,
Photoinitiator, moisturizer, mould inhibitor, cooling agent, water are mixed to get cold compress water-setting collagen solution；The crosslinking agent is acrylate
Crosslinking agent；
(3) cold compress that step (2) obtains continuously is coated on base material, and on coating machine through ultraviolet lighting with water-setting collagen solution
Curing gel is cut it, is packed up to hydrogel plaster product.
2. the preparation method of cold compress hydrogel plaster according to claim 1, which is characterized in that step (1) specifically includes：
(1-1) starts in polyethylene glycol, reaction kettle of the polyvinyl alcohol input with water knockout drum and condenser blender, heats
To 90~95 DEG C, insulated and stirred is complete to polyvinyl alcohol dissolving；
(1-2) and then 50~60 DEG C are cooled to, addition acrylic acid, water entrainer, polymerization inhibitor, catalyst are heated to reaction system and go out
Existing backflow phenomenon, and maintain to be reacted at this temperature；
(1-3) reaction terminates, and is cooled to 40 DEG C hereinafter, being filtered to remove solid catalyst, recycling design obtains polyethylene glycol, gathers
Vinyl alcohol-acrylic acid mixed ester.
3. the preparation method of cold compress hydrogel plaster according to claim 2, which is characterized in that according to weight percent
It counts, raw material includes in the step (1)：
Raw material includes in the step (2)：
4. the preparation method of the cold compress hydrogel plaster according to Claims 2 or 3, which is characterized in that the crosslinking agent
Including one or both of glycol diacrylate, trimethylolpropane trimethacrylate, pentaerythritol triacrylate
Object mixed above.
5. the preparation method of the cold compress hydrogel plaster according to Claims 2 or 3, which is characterized in that described is light-initiated
Agent includes one or more of benzoin methyl ether, benzoin ethyl ether, dihydroxy benaophenonel mixture.
6. the preparation method of the cold compress hydrogel plaster according to Claims 2 or 3, which is characterized in that the water entrainer
Including one or more of benzene,toluene,xylene mixture；The polymerization inhibitor includes hydroquinone, tert-butyl o
One or more of benzenediol, p-hydroxyanisole mixture；The catalyst is urged for the solid acid of esterification
Agent.
7. according to the preparation method of the cold compress hydrogel plaster described in Claims 2 or 3, which is characterized in that the aqueous tackifier
Resin includes one or more of polyvinylpyrrolidone, sodium carboxymethylcellulose, hydroxyethyl cellulose mixture.
8. according to the preparation method of the cold compress hydrogel plaster described in Claims 2 or 3, which is characterized in that the moisturizer packet
Include one or more of the polyalcohols such as glycerine, propylene glycol, butanediol mixture.
9. the preparation method of the cold compress hydrogel plaster described in Claims 2 or 3, which is characterized in that the mould inhibitor includes
One or more of sodium benzoate, potassium sorbate, parabens mould inhibitor mixture；The cooling agent includes nothing
One or more of water-ethanol, medicinal alcohol, Peppermint essential oil etc. mixture.
10. a kind of cold compress hydrogel plaster, which is characterized in that by claim 1~9 any one of them cold compress hydrogel plaster
Preparation method be prepared.
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| CN201711400373.8A CN108159023A (en) | 2017-12-22 | 2017-12-22 | A kind of preparation method and product of cold compress hydrogel plaster |
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| CN201711400373.8A CN108159023A (en) | 2017-12-22 | 2017-12-22 | A kind of preparation method and product of cold compress hydrogel plaster |
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Application publication date: 20180615 |