CN102585273A - Preparation method of high-expansion liquid absorption sponge - Google Patents
Preparation method of high-expansion liquid absorption sponge Download PDFInfo
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- CN102585273A CN102585273A CN201210005124XA CN201210005124A CN102585273A CN 102585273 A CN102585273 A CN 102585273A CN 201210005124X A CN201210005124X A CN 201210005124XA CN 201210005124 A CN201210005124 A CN 201210005124A CN 102585273 A CN102585273 A CN 102585273A
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Abstract
The invention relates to a preparation method of a high-expansion liquid absorption sponge, which belongs to the field of preparation of biomedical materials. The preparation method comprises the following steps of: mixing two polyvinyl formal reaction solutions with different degrees of reaction, then reacting continuously and performing pouring, curing, demolding, cleaning and other steps for getting a final product. According to the preparation method disclosed by the invention, polyvinyl formal with higher depth of pre-reaction is utilized for making a hole-forming core so as to prepare a sponge material, and the material has the characteristics of regular hole structure, no residue of foreign matters, soft texture, immediate expansion when the material meets with water and the like, and is suitable for surgical hematophagia, liquid absorption and other purposes in the medical field.
Description
Technical field
The invention belongs to field of biomedical materials, relate to the preparation method of a kind of high expansion imbibition sponge.
Background technology
Often in the surgical operation adopt traditional medical yarn, limited and rate of liquid aspiration is slow because of its liquid absorption, especially there is to fall the danger of bits, in clinical application, receive certain limitation.Upgrading substitute as traditional medical yarn; High expansion medical sponge is very general in the application of western developed country, and typical product is from U.S. merocel company, and its material is Z 150PH (PVA) sponge; It has good biocompatibility, rate of liquid aspiration is fast and liquid absorption big, Stability Analysis of Structures is not fallen bits; Material softness, plurality of advantages such as tactility is comfortable can be used for the filling of postoperative nasal sinus, ophthalmologic operation is sucked blood and drainage, Neurological Surgery and negative pressure drainage trauma care etc.
The most classical in the PVA sponge production technology is starch pore method; Its method is in the reaction solution of polyvinyl alcohol water solution, formaldehyde and mineral acid, to add starch; Starch expands in PVF crosslinking curing process and disintegrates; It occupies the position and forms hole, and flush away promptly gets spongy mass after disintegrating thing and other material.Usually the starch detritus is to be difficult to thoroughly clean, and chance wet condition spongy mass is very easy to be mouldy.It is very strict that medical sponge requires, and therefore generally can not take this method to produce.
It is other a kind of method of preparation PVA sponge that introducing gas foams; A kind of polyvinyl alcohol foam material for medical sanitation and method for making thereof are disclosed like patent CN94102999.9; Adopt sodium hydrogencarbonate to make whipping agent, but it does not provide the performance and the structural parameter of gained material.Utilize the foam theory of tensio-active agent to prepare other a kind of mode that the PVA sponge is the gas foaming method, it relies on the mechanical stirring method to blast air, under influence of surfactant, forms the foam of certain degree of stability.Patent CN101613512A discloses a kind of imbibing foamed material and preparation method thereof, and used tensio-active agent is selected T 46155 mountain plough sugar alcohol acid anhydride mono-laurate and sodium lauryl sulphate etc. for use.In water react liquid, foam, note foamy stability, the control of cell uniformity at this moment has very highly difficult, and its enforcement has certain limitation.
Summary of the invention
The objective of the invention is to aim to provide a kind of starch based pore-creating agent that do not need, also do not prepare the novel clean preparation method of the high expansion imbibition of PVA sponge through gas or tensio-active agent foaming.The mixed reaction solution of polyvinyl alcohol water solution, formaldehyde and the mineral acid that it is characterized in that two bursts of acetalation degree there are differences mixes the continued reaction by a certain percentage; Regulate the size and the flexibility in material aperture through the relative add-on that changes two strands of materials.The sponge drying that adopts this method to make be compressed to its volume about 20% after, meet that 25 ℃ saline water can expand and softening in 1 second.
Different with the method that prepared PVA sponge or porous material in the past; The present invention utilizes self material pore-forming in reaction process; It comes down to the pore former of the higher PVF of the pre-reaction degree of depth as the PVA sponge, and its principle is in two liquid blended subsequent reactions processes, owing to there is the difference on the level of response; The higher preferential phase-splitting of PVF of the pre-reaction degree of depth is separated out from the aqueous solution, and it has served as and in whole material, plays the pore-forming core.
Preparing method of the present invention is characterized in that may further comprise the steps.
(1) under the temperature more than 80 ℃, PVA-1799 is dissolved in water fully, under 40～70 ℃ of temperature, adds hydrochloric acid and formaldehyde then, reacted 20～60 minutes, get feed liquid A.The weight percentage of each raw material is: PVA-1799 is 4 ~ 12%, hydrochloric acid 2 ~ 10%, and formaldehyde 2 ~ 12%, surplus is a water.
(2) under the temperature more than 80 ℃, polyvinyl alcohol resin is dissolved in water fully, under 40～70 ℃ of temperature, adds hydrochloric acid and formaldehyde then, reacted 0～20 minute, get feed liquid B.The weight percentage of each raw material: PVA-1799 is 4 ~ 12%, hydrochloric acid 2 ~ 10%, and formaldehyde 2 ~ 12%, surplus is a water.
(3) feed liquid A and feed liquid B maintain the temperature at 40～70 ℃ by weight the mixed of 1:5～100, continue to stir 5～60 minutes.
(4) the reacted feed liquid of step (3) is poured in the mould, placed baking oven to be incubated 10～24 hours down in 50～70 ℃.Through the demoulding, clean, obtain clean spongy mass.
Prepared its aperture of sponge of the present invention is between 0.1～2.0mm, and quality is soft, drying be compressed to its original thickness about 20% after, meets 25 ℃ saline water fluid power and in 1 second, expands and soften.
The present invention has following characteristics.
1, reaction feed liquid of the present invention is the homogeneous phase material, good fluidity, and easily cast, and gained PVA sponge product aperture structure is even, quality is soft, and the gas foaming legal system is equipped with and notes foamy stability in the process, the control of cell uniformity also has very highly difficult.
2, the adding starch pore method technology with traditional is different; The present invention arrives the pore former of the PVF of certain depth as the PVA sponge with pre-reaction; There is not foreign matter; Clean simply, solved starch in the previous methods and be difficult to the problem that thoroughly from sponge, cleans up, the gained sponge product is fit to do medical material.
The preparation method that the present invention adopted is simple, and gained PVA sponge has meets water and expands immediately, and quality is soft, and liquid absorption is big, and retained foreign body does not fall characteristics such as bits, suitable medical field do surgery with suck blood, purposes such as imbibition.
Embodiment
The present invention will be described further through following examples.
Embodiment 1.
In the there-necked flask that band stirs, add 5gPVA-1799 and 50 g water, be heated to 85 ℃ to molten fully clear.Cool the temperature to 60 ℃ then, (mass percent, down together) hydrochloric acid of adding 15 g18% under whipped state and 5 g 37% (mass percent, down together) formalin, reaction is 50 minutes under 60 ℃.
In another there-necked flask, add 50gPVA-1799 and 500 g water, heating for dissolving cools the temperature to 60 ℃ then to clear, under whipped state, adds 150 g18% hydrochloric acid and 50 g, 37% formalin.Continue down to stir 2 minutes at 60 ℃.
Above-mentioned two feed liquids are mixed, continue to react 10 minutes down at 60 ℃.
The feed liquid that reaction is good is poured in the mould, places baking oven in 65 ℃ of insulations 12 hours down, and the demoulding is then cleaned, and obtains clean spongy mass, cuts into the sample of specified shape after freezing below 0 ℃, and its specification is long 8cm, wide 2cm, thick 1.5cm.
Sample is made morphology observation with opticmicroscope after drying, the result shows its aperture between 0.1～0.5 mm, and pore distribution is regular.
The mensuration of liquid absorption is undertaken by weighting method, and the imbibition object is 25 ℃ a water.Liquid absorption is calculated as follows:
In the formula
QBe liquid absorbency rate,
m 1Be the weight (g) of sponge sample before the imbibition,
m 2Weight (g) for sponge sample after the imbibition.
Through measuring, liquid absorption is 15 times of spongy mass own wt.
The measuring method of speed of expansion: sample is compressed to thick 3mm, inserts in 25 ℃ the physiological salt liquid, keep for some time after, take out and observe.The result shows that this sponge sample can expand rapidly in the 1s clock softening, returns to the size under original wet condition.
Embodiment 2.
In the there-necked flask that band stirs, add 5gPVA-1799 and 50 g water, be heated to 85 ℃ to molten fully clear.Cool the temperature to 60 ℃ then, under whipped state, add 15 g18% hydrochloric acid and 4.5 g, 37% formalin, reacted 50 minutes down at 60 ℃.
In another there-necked flask, add 50gPVA-1799 and 500 g water, heating for dissolving cools the temperature to 60 ℃ then to clear, under whipped state, adds 150 g18% hydrochloric acid and 45 g, 37% formalin.Continue down to stir 10 minutes at 60 ℃.
Above-mentioned two feed liquids are mixed, continue to react 20 minutes down at 60 ℃.
The feed liquid that reaction is good is poured in the mould, places baking oven in 65 ℃ of insulations 12 hours down, and the demoulding is then cleaned, and obtains clean spongy mass, cuts into the sample of specified shape after freezing below 0 ℃, and its specification is long 8cm, wide 2cm, thick 1.5cm.
Sample is made morphology observation with opticmicroscope after drying, the result shows its aperture between 0.2～1.0 mm, and pore distribution is regular.
Through measuring, its liquid absorption is 15 times of spongy mass own wt, and this sponge is compressed to the saline water fluid power of meeting 25 ℃ behind the thick 3mm and in the 1s clock, expands softeningly rapidly, returns to the size under original wet condition.
Embodiment 3.
In the there-necked flask that band stirs, add 5gPVA-1799 and 60 g water, be heated to 85 ℃ to molten fully clear.Cool the temperature to 50 ℃ then, under whipped state, add 16 g18% hydrochloric acid and 5 g, 37% formalin, reacted 50 minutes down at 50 ℃.
In another there-necked flask, add 100gPVA-1799 and 1200 g water, heating for dissolving cools the temperature to 50 ℃ then to clear, under whipped state, adds 320 g18% hydrochloric acid and 100 g, 37% formalin.Continue down to stir 10 minutes at 50 ℃.
Above-mentioned two feed liquids are mixed, continue to react 20 minutes down at 50 ℃.
The feed liquid that reaction is good is poured in the mould, places baking oven in 65 ℃ of insulations 11 hours down, and the demoulding is then cleaned, and obtains clean spongy mass, cuts into the sample of specified shape after freezing below 0 ℃, and its specification is long 8cm, wide 2cm, thick 1.5cm.
Sample is made morphology observation with opticmicroscope after drying, the result shows its aperture between 0.5～2.0 mm, and pore distribution is regular.
Through measuring, its liquid absorption is 16 times of spongy mass own wt, and this sponge is compressed to the saline water fluid power of meeting 25 ℃ behind the thick 3mm and in the 1s clock, expands softeningly rapidly, returns to the size under original wet condition.
Embodiment 4.
In the there-necked flask that band stirs, add 5g PVA-1799 and 70 g water, be heated to 85 ℃ to molten fully clear.Cool the temperature to 60 ℃ then, under whipped state, add 20 g18% hydrochloric acid and 6 g, 37% formalin, reacted 45 minutes down at 60 ℃.
In another there-necked flask, add 200gPVA-1799 and 2800 g water, heating for dissolving cools the temperature to 60 ℃ then to clear, under whipped state, adds 800 g18% hydrochloric acid and 240 g, 37% formalin.Continue down to stir 6 minutes at 60 ℃.
Above-mentioned two feed liquids are mixed, continue reacting 6 minutes down at these 60 ℃.
The feed liquid that reaction is good is poured in the mould, places baking oven in 60 ℃ of insulations 17 hours down, and the demoulding is then cleaned, and obtains clean spongy mass, cuts into the sample of specified shape after freezing below 0 ℃, and its specification is long 8cm, wide 2cm, thick 1.5cm.
Sample is made morphology observation with opticmicroscope after drying, the result shows its aperture between 0.2～1.0 mm, and pore distribution is regular.
Through measuring, its liquid absorption is 19 times of spongy mass own wt, and this sponge is compressed to the saline water fluid power of meeting 25 ℃ behind the thick 3mm and in the 1s clock, expands softeningly rapidly, returns to the size under original wet condition.
Claims (1)
1. the preparation method of one kind high expansion imbibition sponge is characterized in that may further comprise the steps:
(1) under the temperature more than 80 ℃, PVA-1799 is dissolved in water fully, under 40～70 ℃ of temperature, adds hydrochloric acid and formaldehyde then, reacted 20～60 minutes, get feed liquid A;
The weight percentage of each raw material is: PVA-1799 is 4 ~ 12%, hydrochloric acid 2 ~ 10%, and formaldehyde 2 ~ 12%, surplus is a water;
(2) under the temperature more than 80 ℃, polyvinyl alcohol resin is dissolved in water fully, under 40～70 ℃ of temperature, adds hydrochloric acid and formaldehyde then, reacted 0～20 minute, get feed liquid B;
The weight percentage of each raw material: PVA-1799 is 4 ~ 12%, hydrochloric acid 2 ~ 10%, and formaldehyde 2 ~ 12%, surplus is a water;
(3) feed liquid A and feed liquid B maintain the temperature at 40～70 ℃ by weight the mixed of 1:10～100, continue to stir 5～60 minutes;
(4) the reacted feed liquid of step (3) is poured in the mould, placed baking oven to be incubated 10～24 hours down in 50～70 ℃; Through the demoulding, clean, obtain clean spongy mass.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107349460A (en) * | 2017-07-05 | 2017-11-17 | 吴桂生 | A kind of department of anesthesia's medical sthptic sponge and preparation method thereof |
| CN107903428A (en) * | 2017-11-02 | 2018-04-13 | 阿不力克木 | preparation method of medical polyvinyl alcohol sponge |
| CN108126233A (en) * | 2017-12-28 | 2018-06-08 | 广州润虹医药科技股份有限公司 | A kind of highly expanded rate compressed sponge |
| CN109481151A (en) * | 2018-12-18 | 2019-03-19 | 孙震 | A kind of medical imbibition cotton process units and medical imbibition cotton production system |
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| CN101954115A (en) * | 2010-10-22 | 2011-01-26 | 佘振定 | Medical antibacterial sponge dressing and preparation method thereof |
| CN101967254A (en) * | 2010-10-22 | 2011-02-09 | 佘振定 | Medicinal microporous sponge and preparation method thereof |
| CN102020816A (en) * | 2010-11-16 | 2011-04-20 | 谭明宁 | Polyvinyl formal sponge material with uniform abscesses and rapid imbibition and preparation method thereof |
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- 2012-01-10 CN CN201210005124.XA patent/CN102585273B/en not_active Expired - Fee Related
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| CN101829353A (en) * | 2009-03-10 | 2010-09-15 | 陕西杨凌岱鹰生物技术研究所 | Medical sthptic sponge and preparation method thereof |
| CN101954115A (en) * | 2010-10-22 | 2011-01-26 | 佘振定 | Medical antibacterial sponge dressing and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107349460A (en) * | 2017-07-05 | 2017-11-17 | 吴桂生 | A kind of department of anesthesia's medical sthptic sponge and preparation method thereof |
| CN107903428A (en) * | 2017-11-02 | 2018-04-13 | 阿不力克木 | preparation method of medical polyvinyl alcohol sponge |
| CN108126233A (en) * | 2017-12-28 | 2018-06-08 | 广州润虹医药科技股份有限公司 | A kind of highly expanded rate compressed sponge |
| CN109481151A (en) * | 2018-12-18 | 2019-03-19 | 孙震 | A kind of medical imbibition cotton process units and medical imbibition cotton production system |
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| CN102585273B (en) | 2014-04-09 |
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