CN105111947A - Preparation method of medical instant adhesive - Google Patents
Preparation method of medical instant adhesive Download PDFInfo
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- CN105111947A CN105111947A CN201510534677.8A CN201510534677A CN105111947A CN 105111947 A CN105111947 A CN 105111947A CN 201510534677 A CN201510534677 A CN 201510534677A CN 105111947 A CN105111947 A CN 105111947A
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Abstract
The invention discloses a preparation method of a medical instant adhesive, which comprises the following steps: adding 2-7 parts by weight of butyl rubber, 7-10 parts by weight of ester gum, 1-5 parts by weight of polyethyleneglycol, 1-3 parts by weight of calcium lignosulphonate and 2-4 parts by weight of sodium alginate into a stirrer, stirring uniformly, adding 2-5 parts by weight of diethyl phosphite and 3-7 parts of chlorinated paraffin, uniformly mixing, compounding, adding 2-5 parts by weight of maleamic acid and 3-6 parts by weight of methacrylic acid, stirring for 30-50 minutes while heating in the presence of inert gas, and compounding to obtain the medical instant adhesive. The appropriate process control and component addition and proportioning are performed to obtain the medical instant adhesive which has the advantages of short curing time, high adhesiveness, high stripping property and favorable water resistance, thereby further widening the applicability of the instant adhesive.
Description
Technical field
The invention belongs to medical macromolecular materials technical field, be specifically related to a kind of preparation method of medical instant drying adhesive.
Background technology
Namely moment then uses glue to the solid name Si Yi of instant drying adhesive fast, and conventional is based on ethyl α-cyanoacrylate, adds tackifier, thickening material, stablizer, toughner, stopper etc., the single-component fast setting tackiness agent synthesized by vanguard technology; A kind of high strength, quick tackiness agent, the high short-term training that can be used in multiple types material proceeds with one's work, and is particularly suitable for being used in woodenware industry; For fitting tightly, porous material, such as rubber, metal, plastic cement, woodenware etc. can reach the strongest then effect; This glue is a single composition, solvent-free, does not need the tackiness agent adding catalyst, heating or pressurization, only needs meagre one deck glue, and it just can utilize the atmospheric moisture in air to produce high polymeric, and what reach the best amplexiforms effect.Have natural adhesive and synthetic adhesive point, also can be divided into organic adhesion agent and inorganic adhesive.Alpha-cyanoacrylate ester gum is single component, low viscosity, transparent, normal temperature fast setting tackiness agent.Gluing of surfaces, has good cementability to most material, is one of important room temperature setting adhesives kind.Weak point is that speed of response is too fast, and water tolerance is poor, and fragility is large, and heatproof is low, and preservation period is short, and weather resistance is bad, therefore will add people's corresponding auxiliary agent when joining glue, is used for provisional bonding.Material of main part is specific cyanoacrylate, then adds some auxiliary substances as stablizer, thickening material, softening agent, stopper etc.Should exclusion of water steam as far as possible when joining glue, it is little or air-locked that packaging vessel also applies ventilation property.The most frequently used base-material of response type acrylic ester adhesive is methyl methacrylate.In the medical field, due to the singularity of working conditions, often better requirement is proposed to the performance of instant drying adhesive, as gluing is shorter for set time, gumminess is better, and rippability is higher, water tolerance is better, therefore needs to develop the better instant drying adhesive of a kind of performance and meets use needs.
Summary of the invention
The object of the invention is to overcome above the deficiencies in the prior art and the preparation method that provides a kind of medical instant drying adhesive, the instant drying adhesive that the method obtains has solidification rapidly, the feature of rippability and water-tolerant.
The present invention is realized by following technique means:
A preparation method for medical instant drying adhesive, step is as follows:
Step one, by with isoprene-isobutylene rubber 2-7 part of parts by weight, ester gum 7-10 part, polyoxyethylene glycol 1-5 part, calcium lignin sulphonate 1-3 part, sodium alginate 2-4 part joins in stirrer and is uniformly mixed, and obtains material one;
Step 2, adds diethyl phosphite 2-5 part and clorafin 3-7 part, carries out mixing, obtain mixing thing after mixing in material one;
Step 3, adds maleinamic acid 2-5 part in mixing thing, methacrylic acid 3-6 part, heated and stirred 30-50 minute in the presence of an inert gas, and then carries out mixing, obtains medical instant drying adhesive.
The preparation method of described medical instant drying adhesive, the stirring velocity be uniformly mixed in step one is 100-120 rev/min, churning time 20-30 minute.
The preparation method of described medical instant drying adhesive, melting temperature mixing in step 2 is 130-140 DEG C, mixing time 30-50 minute.
The preparation method of described medical instant drying adhesive, in step 3, rare gas element is nitrogen or argon gas.
The preparation method of described medical instant drying adhesive, temperature mixing in step 3 is 140-150 DEG C, and mixing time is 20-30 minute.
The preparation method of described medical instant drying adhesive, in step 3, the temperature of heated and stirred is 70-80 DEG C.
Within medical instant drying adhesive provided by the invention reaches 36s set time, stripping strength reaches 0.15KNm
-1having excellent water-resistance in the water of 50 DEG C after 12h, not there is exception in performance, peel off integrity and reach more than 99.6%, shearing resistance reaches more than 15MPa, has good bond properties and water tolerance, and set time is short simultaneously, separability is good, can apply to medical field more widely.
Embodiment
Embodiment 1
A preparation method for medical instant drying adhesive, step is as follows:
Step one, by with the isoprene-isobutylene rubber 2 parts of parts by weight, ester gum 7 parts, polyoxyethylene glycol 1 part, calcium lignin sulphonate 1 part, sodium alginate 2 parts joins in stirrer and is uniformly mixed, stirring velocity is 100 revs/min, and churning time 20 minutes, obtains material one;
Step 2, in material one, add diethyl phosphite 2 parts and clorafin 3 parts, carry out mixing after mixing, melting temperature is 130 DEG C, and mixing time 30 minutes, obtains mixing thing;
Step 3, adds maleinamic acid 2 parts in mixing thing, and methacrylic acid 3 parts, deposits at nitrogen and be heated to 70-80 DEG C in case, and stir 30 minutes, and then carry out mixing, mixing temperature is 140 DEG C, and mixing time is 20 minutes, obtains medical instant drying adhesive.
Embodiment 2
A preparation method for medical instant drying adhesive, step is as follows:
Step one, by with the isoprene-isobutylene rubber 2 parts of parts by weight, ester gum 8 parts, polyoxyethylene glycol 2 parts, calcium lignin sulphonate 1 part, sodium alginate 3 parts joins in stirrer and is uniformly mixed, stirring velocity is 105 revs/min, and churning time 23 minutes, obtains material one;
Step 2, in material one, add diethyl phosphite 3 parts and clorafin 4 parts, carry out mixing after mixing, melting temperature is 133 DEG C, and mixing time 38 minutes, obtains mixing thing;
Step 3, adds maleinamic acid 3 parts in mixing thing, and methacrylic acid 4 parts is deposited at argon gas and is heated to 75 DEG C in case, and stir 36 minutes, and then carry out mixing, mixing temperature is 142 DEG C, and mixing time is 25 minutes, obtains medical instant drying adhesive.
Embodiment 3
A preparation method for medical instant drying adhesive, step is as follows:
Step one, by with the isoprene-isobutylene rubber 5 parts of parts by weight, ester gum 8 parts, polyoxyethylene glycol 4 parts, calcium lignin sulphonate 2 parts, sodium alginate 4 parts joins in stirrer and is uniformly mixed, stirring velocity is 110 revs/min, and churning time 28 minutes, obtains material one;
Step 2, in material one, add diethyl phosphite 4 parts and clorafin 5 parts, carry out mixing after mixing, melting temperature is 138 DEG C, and mixing time 42 minutes, obtains mixing thing;
Step 3, adds maleinamic acid 4 parts in mixing thing, and methacrylic acid 5 parts is deposited at nitrogen and is heated to 78 DEG C in case, and stir 45 minutes, and then carry out mixing, mixing temperature is 146 DEG C, and mixing time is 28 minutes, obtains medical instant drying adhesive.
Embodiment 4
A preparation method for medical instant drying adhesive, step is as follows:
Step one, by with the isoprene-isobutylene rubber 7 parts of parts by weight, ester gum 10 parts, polyoxyethylene glycol 5 parts, calcium lignin sulphonate 3 parts, sodium alginate 4 parts joins in stirrer and is uniformly mixed, stirring velocity is 120 revs/min, and churning time 30 minutes, obtains material one;
Step 2, in material one, add diethyl phosphite 5 parts and clorafin 7 parts, carry out mixing after mixing, melting temperature is 140 DEG C, and mixing time 50 minutes, obtains mixing thing;
Step 3, adds maleinamic acid 5 parts in mixing thing, and methacrylic acid 6 parts is deposited at nitrogen and is heated to 80 DEG C in case, and stir 50 minutes, and then carry out mixing, mixing temperature is 150 DEG C, and mixing time is 30 minutes, obtains medical instant drying adhesive.
Comparative example 1
A preparation method for medical instant drying adhesive, step is as follows:
Step one, by with the isoprene-isobutylene rubber 5 parts of parts by weight, ester gum 8 parts, polyoxyethylene glycol 4 parts, calcium lignin sulphonate 2 parts, sodium alginate 4 parts joins in stirrer and is uniformly mixed, stirring velocity is 110 revs/min, and churning time 28 minutes, obtains material one;
Step 2, in material one, add diethyl phosphite 4 parts and clorafin 5 parts, carry out mixing after mixing, melting temperature is 138 DEG C, and mixing time 42 minutes, obtains mixing thing;
Step 3, carrying out mixing, mixing temperature again to mixing thing is 146 DEG C, and mixing time is 28 minutes, obtains medical instant drying adhesive.
Comparative example 2
A preparation method for medical instant drying adhesive, step is as follows:
Step one, by with the isoprene-isobutylene rubber 5 parts of parts by weight, ester gum 8 parts, polyoxyethylene glycol 4 parts, calcium lignin sulphonate 2 parts, sodium alginate 4 parts joins in stirrer and is uniformly mixed, stirring velocity is 110 revs/min, and churning time 28 minutes, obtains material one;
Step 2, adds diethyl phosphite 4 parts and clorafin 5 parts, mixes and obtain mixture in material one;
Step 3, adds maleinamic acid 4 parts in the mixture, and methacrylic acid 5 parts is deposited at nitrogen and is heated to 78 DEG C in case, and stir 45 minutes, and then carry out mixing, mixing temperature is 146 DEG C, and mixing time is 28 minutes, obtains medical instant drying adhesive.
Carry out performance test to above embodiment and the medical instant drying adhesive of comparative example gained, result is as follows:
Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 |
Set time/s | 36 | 28 | 25 | 26 | 31 | 56 |
180 ° of stripping strength/KNm -1 | 0.15 | 0.16 | 0.16 | 0.15 | 0.09 | 0.15 |
Water tolerance (in 50 DEG C of water 12h) | Performance is without exception | Performance is without exception | Performance is without exception | Performance is without exception | Fragility becomes large | Performance is without exception |
Peel off integrity/% | 99.6 | 99.8 | 100 | 99.9 | 96.2 | 99.5 |
Shearing resistance | 15 | 16 | 18 | 16 | 8 | 16 |
As can be seen from the above results, within medical instant drying adhesive provided by the invention reaches 36s set time, stripping strength reaches 0.15KNm
-1having excellent water-resistance in the water of 50 DEG C after 12h, not there is exception in performance, peel off integrity and reach more than 99.6%, shearing resistance reaches more than 15MPa, has good bond properties and water tolerance, and set time is short simultaneously, separability is good, can apply to medical field more widely.
Comparative example 1 and comparative example 2 are the further proving tests carried out on the basis of the embodiment of the present invention 3, wherein in preparation process three, do not add maleinamic acid and methacrylic acid in comparative example 1, there is no reacting by heating under nitrogen existence condition simultaneously, and directly carry out mixing, the instant drying adhesive shearing resistance finally prepared and stripping strength significantly reduce, water tolerance is deteriorated simultaneously, in water, fragility becomes large, therefore can find out, adhesion characteristic and the water tolerance of the finished product can be strengthened by above preparation method; Do not carry out mixing in comparative example 2 in step 2, but be mixed directly and obtain mixture, other processes are identical with embodiment 3, the instant drying adhesive finally obtained is obviously elongated for set time, therefore can illustrate, first time of increase mixing can the curing performance of improving product, shorten set time.As can be seen from the above, the preparation method of medical instant drying adhesive provided by the invention is added and proportioning by suitable process control and component, obtains set time short, binding property and stripping performance high, the medical instant drying adhesive of water-tolerant, has expanded the application of instant drying adhesive further.
Claims (6)
1. a preparation method for medical instant drying adhesive, is characterized in that, step is as follows:
Step one, by with chloroprene rubber 3-8 part of parts by weight, barium stearate 1-3 part, polyoxyethylene glycol 2-7 part, Vltra tears 2-6 part, trevira 3-8 part joins in stirrer and is uniformly mixed, and obtains material one;
Step 2, in material one, add the acrylamide 1-4 part with parts by weight, Secondary ammonium phosphate 2-5 part, is heated to 50-60 DEG C under vacuum, stirs 15-20 minute, obtains reactant one;
Step 3, adds the maleinamic acid 2-6 part with parts by weight in reactant one,
Diethyl phosphite 2-5 part and clorafin 3-7 part, carry out mixing, obtain mixing thing after mixing;
Step 3, adds maleinamic acid 2-5 part in mixing thing, methacrylic acid 3-6 part, heated and stirred 30-50 minute in the presence of an inert gas, and then carries out mixing, obtains medical instant drying adhesive.
2. the preparation method of medical instant drying adhesive according to claim 1, is characterized in that, the stirring velocity be uniformly mixed in step one is 100-120 rev/min, churning time 20-30 minute.
3. the preparation method of medical instant drying adhesive according to claim 1, is characterized in that, melting temperature mixing in step 2 is 130-140 DEG C, mixing time 30-50 minute.
4. the preparation method of medical instant drying adhesive according to claim 1, is characterized in that, in step 3, rare gas element is nitrogen or argon gas.
5. the preparation method of medical instant drying adhesive according to claim 1, is characterized in that, temperature mixing in step 3 is 140-150 DEG C, and mixing time is 20-30 minute.
6. the preparation method of medical instant drying adhesive according to claim 1, is characterized in that, in step 3, the temperature of heated and stirred is 70-80 DEG C.
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CN201510534677.8A CN105111947A (en) | 2015-08-27 | 2015-08-27 | Preparation method of medical instant adhesive |
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CN201510534677.8A CN105111947A (en) | 2015-08-27 | 2015-08-27 | Preparation method of medical instant adhesive |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106236367A (en) * | 2016-08-04 | 2016-12-21 | 湖南慈辉医疗科技有限公司 | A kind of manufacture method of medical ice pad |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103045107A (en) * | 2012-12-14 | 2013-04-17 | 安徽扬帆充气游乐设备制造有限公司 | Boat water resistant adhesive |
CN103694903A (en) * | 2013-12-02 | 2014-04-02 | 南通瑞普埃尔生物工程有限公司 | Instantaneous adhesive and preparation method thereof |
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2015
- 2015-08-27 CN CN201510534677.8A patent/CN105111947A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103045107A (en) * | 2012-12-14 | 2013-04-17 | 安徽扬帆充气游乐设备制造有限公司 | Boat water resistant adhesive |
CN103694903A (en) * | 2013-12-02 | 2014-04-02 | 南通瑞普埃尔生物工程有限公司 | Instantaneous adhesive and preparation method thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106236367A (en) * | 2016-08-04 | 2016-12-21 | 湖南慈辉医疗科技有限公司 | A kind of manufacture method of medical ice pad |
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