CN1082552A - Polyether(poly)urethane, polyurethane bismuth and preparation method thereof and as the stifled material of uterine tube bolt - Google Patents
Polyether(poly)urethane, polyurethane bismuth and preparation method thereof and as the stifled material of uterine tube bolt Download PDFInfo
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- CN1082552A CN1082552A CN 93112102 CN93112102A CN1082552A CN 1082552 A CN1082552 A CN 1082552A CN 93112102 CN93112102 CN 93112102 CN 93112102 A CN93112102 A CN 93112102A CN 1082552 A CN1082552 A CN 1082552A
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- polyurethane
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Abstract
The invention provides the stifled material of a kind of non-aggressive uterine tube bolt, a kind of polyether(poly)urethane is the preparation that contains polyurethane bismuth on basis, and preparation method thereof, by polyethenoxy ether two pure and mild toluene 2,4 vulcabond pass through prepolymerization reaction again with 1, the reaction of 4 chain expansion of succinic acid generates the polyether-type polyurethane, gets polyurethane bismuth as the stifled material of a kind of non-aggressive uterine tube bolt that develops with the bismuth iodide solution mixing system.
Description
The present invention relates to a kind of urethane resin and its production and use field, be particularly related to the stifled material of non-aggressive uterine tube bolt that a kind of birth control uses, have the display capabilities of X ray and based on the preparation method field of the polyurethane bismuth of polyether(poly)urethane.
The stifled material of uterine tube bolt is used for non-operation sexual sterilization operation, and employing is all arranged both at home and abroad, is broadly divided into corrodibility and non-aggressive two big classes.Silver Nitrate phenol and various compound preparation all belong to corrosive medicine, finally cause blocking uterine tube and sterilization because destroy tunica mucosa tubae uterinae generation granulation tissue hyperplasia mechanism.Contract capraldehyde and base polyurethane prepolymer for use as of Methyl 2-cyanoacrylate, silicon rubber, polyvinyl alcohol all belongs to non-corrosive material, all obtained the effect of birth control, but these materials or because the material preparation process complexity, perhaps because the safety issue of material exists potential danger to human body and can not get applying.Therefore study a kind of nontoxic, safe and effective stifled material of uterine tube bolt that is used for non-operation sexual sterilization operation and become urgent task of the present invention.
Purpose of the present invention provides a kind of excellent biological compatibility that has for non-operation sexual sterilization operation exactly, nontoxic, non-corrosiveness, and the quality softness, the uterine tube bolt that is soluble in dehydrated alcohol blocks up the polyether(poly)urethane and the preparation method of material height line style.Another object of the present invention is injected the oviducal X ray development capability that has with regard to the injection system that is easy to that provides a kind of polyether(poly)urethane based on the height line style, is convenient to the preparation polyurethane bismuth and the preparation method of the stifled effect of clinical observation bolt.
The preparation method of the stifled material polyether(poly)urethane of non-aggressive uterine tube bolt of the present invention:
Adopt molecular weight be 2000 polyethenoxy ether two pure and mild toluene 2,4 vulcabond by prepolymerization reaction, generate performed polymer, then performed polymer and chainextender 1,4 butyleneglycol are carried out chain extending reaction, generate the highly polyether(poly)urethane of line style.
The structural formula of height line style polyether(poly)urethane of the present invention is:
The polyether(poly)urethane resin of height line style of the present invention is light yellow translucent solid, has suitable hardness, is dissolved in benzene, acetone solvent, and the limiting viscosity of benzole soln is between 0.085 to 0.110 in the time of 25 ℃.When limiting viscosity was 0.110, molecular-weight average was 10,200 after measured, and such resin has not contained isocyanic ester after measured.It elementary compositionly has the characteristic feature of urethane for C=60.6 to 61.0% H=8.39 to 8.41% N=4.70 to 4.78% infrared absorption spectrum by ultimate analysis.Content of elements in the urethane: plumbous % is less than 0.0005; Arsenic % is less than 0.0005; Chromium % is less than 0.001; Iron % is less than 0.001; Heavy metal is less than 0.0025%.
The preparation method of polyurethane bismuth:
Polyether(poly)urethane of the present invention is dissolved in the organic solvent, and the compound with bismuth is dissolved in solvent in addition, then under agitation both is mixed, and will add the polyurethane solution water precipitating of bismuth then.The polyurethane bismuth water rinse of separating out.The polyurethane bismuth of separating out is bisque soft solid, through rinsing dry the dried glue of polyurethane bismuth.For adapting to the stifled oviducal requirement of bolt, must be with solid polyurethane bismuth fluidify, the employing dehydrated alcohol is a solvent, proportionally the polyurethane bismuth fragment of doing is added in the dehydrated alcohol and goes, make brick-red fluid by warm stirring, be the polyurethane bismuth preparation of polyether(poly)urethane, promptly can be used for clinical through the packing sterilization for the basis.
Consisting of of polyether(poly)urethane bismuth preparation of the present invention:
Composition weight %
Polyether(poly)urethane 54 to 58
Polyurethane bismuth 2.2 to 2.7
The dehydrated alcohol equal amount
Accompanying drawing 2 is X-ray diffractograms of polyurethane bismuth of the present invention.
1 can find out that infrared absorption spectroscopy has the characteristic feature of polyurethane with reference to the accompanying drawings.
2 can find out that x-ray diffraction pattern only presents the basic salt feature of bismuth with reference to the accompanying drawings, and polyurethane is that the amorphous state material does not possess X-ray diffraction.
Polyurethane bismuth preparation as the stifled material of fallopian tubal bolt of the present invention meets the regulation of table 1.
The physicochemical property specification requirement of table 1 polyurethane bismuth preparation
The index name desired value
The brick red of the gelatin nothing caking of outward appearance
The look thick liquid
Solid content % 54 to 58
Bi content % 2.2 to 2.7
Viscosity (40 ℃) Mpa.s 3000-4500
Plumbous (Pb) %≤0.0005
Cadmium (Cd) %≤0.0005
Arsenic (As) %≤0.0005
Chromium (Cr) %≤0.001
Iron (Fe) %≤0.001
Solid content in the table 1 is according to polyurethane bismuth ethanolic soln viscosity and concentration relationship, and solid content is with reference to State Standard of the People's Republic of China 1725-71(88 in the mensuration that 55% left and right sides polyurethane bismuth solution has moderate viscosity solid content) method measure.
The mensuration of viscosity adopts the gauged rotational viscosimeter of viscosity oil standards (NDJ-79) to measure.
It is according in acidic medium that bi content is measured, xylenol orange and Bi
3+Form water-soluble red complex, use the disodium ethylene diamine tetraacetate titration then.
The mensuration of lead, cadmium, arsenic, iron is by the WSS-1 of Ministry of Health of the People's Republic of China standard code.
Polyurethane bismuth preparation biological test result of the present invention meets the requirement of table 2.
The biological test requirement of table 2 polyurethane bismuth preparation
The project name requirement
Sterility test is reactionless
Hemolytic test is reactionless
Irritant test is reactionless
The calorifics test is reactionless
Acute toxicity test is reactionless
The method of biological test in accordance with regulations
The stifled material polyurethane bismuth of the non-aggressive uterine tube bolt that develops of the present invention is by Shandong Province college of traditional Chinese medicine toxicity, pharmacological research, carry out acute toxicity long term toxicity, haemolysis, stimulation pyrogen Ame experiment, toxicological study shows that polyurethane bismuth has excellent biological compatibility, nontoxic, the no mutagenesis of no burn into is the safe material that meets medical requirement.
The stifled material polyurethane bismuth of the non-aggressive uterine tube bolt that develops of the present invention passes through the Shandong Province Science And Technology Institute For Family Planning, it is 88.32%(uterine cavity method that the People's Hospital, Shandong Province analyzes the single job success ratio to the 556 routine clinical datas of being done) and the 94.5%(intubation) visualization ratio is greater than 92%, development can be kept 7 days.
The stifled material of uterine tube bolt of the present invention is the non-aggressive macromolecular compound,, superfoetation research logical for answering provides prerequisite condition, animal experiment show material of the present invention in vivo stable performance toxicological harmless effect and endosalpinx adhesion does not closely take place, can take out uterine tube and have logical again hope.
Embodiment:
Example 1: polyethenoxy ether glycol 360-386 gram, with Toluene-2,4-diisocyanate, 4-vulcabond 187 grams, stirred 2-5 hour down at 80 ℃, carry out pre-polymerization, generate performed polymer, then performed polymer cools off, when the temperature of performed polymer is reduced to 16 to 32 ℃, add 1 of 81 grams, 4 butyleneglycols carry out chain extending reaction, between the temperature of chain extension keeps 30 to 70 ℃, approximately through one hour when temperature of reaction system begins to descend, reactant transfer to the polyethylene film plastics bag, is sealed in the refrigerator that is positioned over-4 ℃, place diel, move to then and place 3 in 4 ℃ the environment round the clock, then at room temperature place six round the clock, under 80 ℃, add thermomaturation 6 hours then, obtain polyether(poly)urethane.
Example 2:
150 gram polyether(poly)urethanes are dissolved in 500 milliliters of (about 400 grams) acetone (second class grade chemical), in addition with 25 gram bismuth iodides (three grades of reagent) and 10 gram potassiumiodides (second class grade chemical), be dissolved in 500 milliliters of dehydrated alcohols (second class grade chemical), under agitation cold polyurethane solution is mixed with bismuth iodide solution then and obtain red polyurethane bismuth solution, then polyurethane bismuth solution is inclined in the water, polyurethane bismuth is separated out, the polyurethane bismuth that obtains is soaked 7 round the clock in water, change water every day once, to remove organic solvent 80 ℃ of following vacuum-dryings three round the clock at last, will obtain the dried glue of polyurethane bismuth with polyurethane bismuth.
The dried peptization of polyurethane bismuth is made solid content in the second class grade chemical dehydrated alcohol be 54 to 58% polyurethane bismuth preparation.
Claims (4)
1, a kind of its structural formula of polyether(poly)urethane resin is:
2, a kind of preparation that contains polyurethane bismuth based on polyether(poly)urethane is characterized in that containing following composition:
Composition weight %
Polyether-polyurethane 54 to 58
Polyurethane bismuth 2.2 to 2.7
The dehydrated alcohol equal amount
3, it is characterized in that as the stifled material of uterine tube bolt according to the said a kind of polyurethane bismuth preparation that contains of claim 2 based on polyether(poly)urethane.
4, the said a kind of preparation that contains polyurethane bismuth based on polyether(poly)urethane according to claim 2 is characterized in that said polyurethane bismuth is as the material with the stifled effect of X ray development capability clinical observation uterine tube bolt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93112102 CN1032818C (en) | 1993-08-11 | 1993-08-11 | Poly ether type polyurethane and polyurethane bismuth, its preparing method and using as oviducal embolism material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93112102 CN1032818C (en) | 1993-08-11 | 1993-08-11 | Poly ether type polyurethane and polyurethane bismuth, its preparing method and using as oviducal embolism material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1082552A true CN1082552A (en) | 1994-02-23 |
| CN1032818C CN1032818C (en) | 1996-09-18 |
Family
ID=4989841
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93112102 Expired - Fee Related CN1032818C (en) | 1993-08-11 | 1993-08-11 | Poly ether type polyurethane and polyurethane bismuth, its preparing method and using as oviducal embolism material |
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| Country | Link |
|---|---|
| CN (1) | CN1032818C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392048B (en) * | 2008-09-27 | 2011-04-27 | 清华大学 | Method for preparing developing polyurethane |
-
1993
- 1993-08-11 CN CN 93112102 patent/CN1032818C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392048B (en) * | 2008-09-27 | 2011-04-27 | 清华大学 | Method for preparing developing polyurethane |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1032818C (en) | 1996-09-18 |
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