CN110982452A - Latex emulsion adhesive with stable mechanical property and preparation method thereof - Google Patents
Latex emulsion adhesive with stable mechanical property and preparation method thereof Download PDFInfo
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- CN110982452A CN110982452A CN201911299040.XA CN201911299040A CN110982452A CN 110982452 A CN110982452 A CN 110982452A CN 201911299040 A CN201911299040 A CN 201911299040A CN 110982452 A CN110982452 A CN 110982452A
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- 239000000853 adhesive Substances 0.000 title claims abstract description 40
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 37
- 239000000839 emulsion Substances 0.000 title claims abstract description 20
- 239000004816 latex Substances 0.000 title claims abstract description 16
- 229920000126 latex Polymers 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 108010022355 Fibroins Proteins 0.000 claims abstract description 33
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002562 thickening agent Substances 0.000 claims abstract description 17
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 10
- 239000000835 fiber Substances 0.000 claims abstract description 9
- 239000004014 plasticizer Substances 0.000 claims abstract description 9
- 239000012745 toughening agent Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 16
- 230000001804 emulsifying effect Effects 0.000 claims description 8
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 8
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 8
- 238000000502 dialysis Methods 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 101000952180 Morus alba Mulatexin Proteins 0.000 abstract description 2
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- 239000013530 defoamer Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 229920001195 polyisoprene Polymers 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J107/00—Adhesives based on natural rubber
- C09J107/02—Latex
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a latex emulsion adhesive with stable mechanical property and a preparation method thereof, wherein the adhesive mainly comprises the following components in parts by weight: 100 parts of natural latex, 4-6 parts of tackifier, 5-6 parts of plasticizer, 0.2-0.6 part of thickener, 0.1-0.3 part of defoaming agent and 1-10 parts of toughening agent, wherein the toughening agent is a regenerated silk fibroin solution prepared from silk powder. Compared with the prior art, the silk fibroin fibers and the natural latex protein are adopted to generate a curing structure, so that the structural stability of the natural latex is enhanced, other auxiliary agents are not easy to crosslink, and the self-bonding of the adhesive is reduced.
Description
Technical Field
The invention relates to a latex emulsion adhesive with stable mechanical property and a preparation method thereof, belonging to the technical field of adhesive preparation.
Background
In recent years, adhesives have been widely used, mainly in the fields of medical treatment, sports equipment, electronics industry, general industry, packaging, and the like, and have been widely used as adhesive portions of articles such as sports protective tapes, bandages, packaging tapes, double-sided tapes, and labels.
The natural latex is a natural high molecular compound which is prepared by filtering and coagulating latex collected from natural plants and takes polyisoprene as a main component. Latex particles of natural latex are essentially polyisoprene as a core surrounded by a non-rubber component shell (e.g., proteins and lipids). From the chemical structure of natural latex, natural latex is nonpolar unsaturated rubber, and the structure is not stable.
CN109777322A discloses a method for improving the self-adhesive property of a natural latex-based adhesive, which relates to a method for improving the self-adhesive property of the natural latex-based adhesive by adding nano particles as a filler into the adhesive, wherein the self-adhesive property of the adhesive is improved by about 160 percent, but the improved mechanical property effect is unstable.
Disclosure of Invention
The purpose of the invention is as follows: in view of the above technical problems, the present invention aims to provide a latex emulsion adhesive with stable mechanical properties and a preparation method thereof, and the obtained adhesive can stabilize the effect while improving the mechanical properties of the latex emulsion adhesive.
The technical scheme is as follows: in order to achieve the purpose, the invention adopts the following technical scheme:
a latex emulsion adhesive mainly comprises the following components in parts by weight:
100 parts of natural latex, 4-6 parts of tackifier, 5-6 parts of plasticizer, 0.2-0.6 part of thickener, 0.1-0.3 part of defoaming agent and 1-10 parts of toughening agent, wherein the toughening agent is a regenerated silk fibroin solution prepared from silk powder.
Preferably, the tackifier is an aqueous tackifying resin XY-8025; the plasticizer is white oil; the thickener is an emulsifying thickener C-580; the defoaming agent is B-422. Preferably, the toughening agent is 1-5 parts.
Preferably, the regenerated silk fibroin solution is mainly prepared by the following steps:
subjecting Tris-SO4Mixing with mercaptoethanol, adding aqueous urea, heating to 70-90 ℃ for reaction, adding silk powder for reaction after the reaction is finished to obtain silk material, washing and air-drying to obtain silk fiber, then adding the silk fiber into an Ajisawa reagent, centrifuging, taking supernatant, and dialyzing in deionized water to obtain the regenerated silk fibroin solution with the concentration of 2-10 wt%.
Further preferably, the Tris-SO4The mol ratio of the mercaptoethanol to the mercaptoethanol is 2 (40-60); the molar ratio of the aqueous urea to the mercapto ethanol is (12-20) to 1; adding silk powder for reaction for 1.5-2.5 hours; the above-mentionedThe components of the Ajisawa reagent are as follows: CaCl2、C2H5OH and H2The molar ratio of O is 1: (1-3): (6-10); the centrifugation conditions were: (7000-9000) rmp centrifugation for 8-12 min; the dialysis is carried out in deionized water, the cut-off value of a dialysis membrane is 5kDa, and the dialysis is carried out for 2-3 days.
The preparation method of the latex emulsion adhesive comprises the following steps:
preparing a toughening agent regenerated silk fibroin solution, mixing natural latex and the regenerated silk fibroin solution at a constant temperature, mixing a plasticizer and a thickening agent, mixing the two mixed solutions, sequentially adding a tackifier and a defoaming agent, mixing each time or adding raw materials, stirring, adding other raw materials, and finally filtering to obtain the silk fibroin composite material.
Preferably, the preparation process comprises the following steps:
mixing the natural latex and the regenerated silk fibroin solution, and stirring for 20-30 minutes;
mixing the plasticizer and the thickening agent, and stirring for 5-10 minutes;
mixing the two mixed solutions, and stirring for 5-10 minutes;
adding the tackifier and stirring for 5-10 minutes;
adding the defoaming agent, and stirring for 2-6 minutes.
Preferably, the constant temperature condition is 40-50 ℃.
The silk fibroin is natural polymer extracted from silk, has excellent characteristics of adhesive force, toughness, biocompatibility, biodegradability and thermal stability, is one of the most widely used natural protein fibers, and has performance superior to that of artificial synthetic fibers and natural fibers. The silk fibroin modified natural latex is used as a base material and added into the adhesive, so that the stability of the natural latex is effectively improved, the stability of the adhesive is further enhanced, and the mechanical property of the adhesive is improved to a certain extent.
The technical effects are as follows: compared with the prior art, the invention has the advantages that: the silk fibroin fiber and the natural latex protein generate a curing structure, so that the structural stability of the natural latex is enhanced, other auxiliary agents are not easy to crosslink, and the self-bonding of the adhesive is reduced.
Drawings
FIG. 1 is a graph showing the results of peel strength measurements of the adhesives prepared in accordance with the present invention.
Detailed Description
The technical solution of the present invention is further described in detail by the following specific examples.
Example 1
100g of natural latex and 1.0g of regenerated silk fibroin solution are put into a stirring kettle at the temperature of 40 ℃ and stirred for 30 minutes at constant temperature, and the natural latex-regenerated silk fibroin mixed emulsion is prepared. 5.0g of white oil and 0.5g of emulsifying thickener C-580 are put into a beaker, stirred for 5 minutes at the constant temperature of 40 ℃, poured into a stirring kettle, continuously stirred for 5 minutes at the constant temperature, added with 4.0g of waterborne tackifying resin XY-8025, stirred for 5 minutes, added with 0.15g of defoamer B-422, stirred for 5 minutes, stirred completely and filtered to obtain the finished adhesive.
Example 2
And (3) putting 100g of natural latex and 2.0g of regenerated silk fibroin solution into a stirring kettle at the temperature of 40 ℃, and stirring for 30 minutes at constant temperature to prepare the natural latex-regenerated silk fibroin mixed emulsion. 5.0g of white oil and 0.5g of emulsifying thickener C-580 are put into a beaker, stirred for 5 minutes at the constant temperature of 40 ℃, poured into a stirring kettle, continuously stirred for 5 minutes at the constant temperature, added with 4.0g of waterborne tackifying resin XY-8025, stirred for 5 minutes, added with 0.15g of defoamer B-422, stirred for 5 minutes, stirred completely and filtered to obtain the finished adhesive.
Example 3
And (3) putting 100g of natural latex and 3.0g of regenerated silk fibroin solution into a stirring kettle at the temperature of 40 ℃, and stirring for 30 minutes at constant temperature to prepare the natural latex-regenerated silk fibroin mixed emulsion. 5.0g of white oil and 0.5g of emulsifying thickener C-580 are put into a beaker, stirred for 5 minutes at the constant temperature of 40 ℃, poured into a stirring kettle, continuously stirred for 5 minutes at the constant temperature, added with 4.0g of waterborne tackifying resin XY-8025, stirred for 5 minutes, added with 0.15g of defoamer B-422, stirred for 5 minutes, stirred completely and filtered to obtain the finished adhesive.
Example 4
And (3) putting 100g of natural latex and 4.0g of regenerated silk fibroin solution into a stirring kettle at the temperature of 40 ℃, and stirring for 30 minutes at constant temperature to prepare the natural latex-regenerated silk fibroin mixed emulsion. 5.0g of white oil and 0.5g of emulsifying thickener C-580 are put into a beaker, stirred for 5 minutes at the constant temperature of 40 ℃, poured into a stirring kettle, continuously stirred for 5 minutes at the constant temperature, added with 4.0g of waterborne tackifying resin XY-8025, stirred for 5 minutes, added with 0.15g of defoamer B-422, stirred for 5 minutes, stirred completely and filtered to obtain the finished adhesive.
Example 5
And (3) putting 100g of natural latex and 5.0g of regenerated silk fibroin solution into a stirring kettle at the temperature of 40 ℃, and stirring for 30 minutes at constant temperature to prepare the natural latex-regenerated silk fibroin mixed emulsion. 5.0g of white oil and 0.5g of emulsifying thickener C-580 are put into a beaker, stirred for 5 minutes at the constant temperature of 40 ℃, poured into a stirring kettle, continuously stirred for 5 minutes at the constant temperature, added with 4.0g of waterborne tackifying resin XY-8025, stirred for 5 minutes, added with 0.15g of defoamer B-422, stirred for 5 minutes, stirred completely and filtered to obtain the finished adhesive.
The preparation method of the regenerated silk fibroin solution described in the above example is as follows:
tris (Tris-hydroxymethyl-aminomethane) -SO with a molar ratio of 2:50 was added to a three-necked flask equipped with a stirrer, a condenser and a thermometer4And mercaptoethanol with the molar ratio of the aqueous urea to the mercaptoethanol of 16:1, heating the system to 80 ℃, adding silk powder, and continuously heating at the constant temperature of 80 ℃ for 2 hours. The resulting silk material was repeatedly washed in deionized water and then air-dried. The resulting silk fibers were added to Ajisawa reagent (CaCl)2/C2H5OH/H2O, 1: 2: 8 molar ratio), the resulting fibroin/salt solution was centrifuged at 8000rmp for 10 minutes. And dialyzing the supernatant with deionized water for 72 hours (the cut-off value of a dialysis membrane is 5kDa), thus obtaining 6 wt% Silk Fibroin (SF) solution.
Comparative example 1 the data were obtained as per the procedure in the example under publication number CN 109777322A;
comparative example 2
5.0g of white oil and 0.5g of emulsifying thickener C-580 are put into a beaker, stirred for 5 minutes at the constant temperature of 40 ℃, poured into a stirring kettle, added with 100g of natural latex and continuously stirred for 10 minutes at the constant temperature of 40 ℃. And adding 0.15g of defoaming agent B-422, stirring for 5 minutes, and filtering to obtain the adhesive.
The peel strength of the invention is detected according to GB/T2791-1995 standard, the detection result is shown in figure 1, and the figure shows that the invention improves the mechanical property of the rubber pressure-sensitive adhesive to a certain extent, and can stabilize the effect within a certain limit, and the additive components are nontoxic, pollution-free and harmless to human bodies.
Claims (7)
1. The latex emulsion adhesive is characterized by mainly comprising the following components in parts by weight:
100 parts of natural latex, 4-6 parts of tackifier, 5-6 parts of plasticizer, 0.2-0.6 part of thickener, 0.1-0.3 part of defoaming agent and 1-10 parts of toughening agent, wherein the toughening agent is a regenerated silk fibroin solution prepared from silk powder.
2. The latex-based emulsion adhesive according to claim 1, wherein said tackifier is an aqueous tackifier resin XY-8025; the plasticizer is white oil; the thickener is an emulsifying thickener C-580; the defoaming agent is B-422.
3. The latex-based emulsion adhesive according to claim 1, wherein the regenerated silk fibroin solution is mainly prepared by the steps of:
subjecting Tris-SO4Mixing with mercaptoethanol, adding aqueous urea, heating to 70-90 ℃ for reaction, adding silk powder for reaction after the reaction is finished to obtain silk material, washing and air-drying to obtain silk fiber, then adding the silk fiber into an Ajisawa reagent, centrifuging, taking supernatant, and dialyzing in deionized water to obtain the regenerated silk fibroin solution with the concentration of 2-10 wt%.
4. The latex emulsion adhesive according to claim 3, wherein said Tris-SO4And of mercaptoethanolThe molar ratio is 2 (40-60); the molar ratio of the aqueous urea to the mercapto ethanol is (12-20) to 1; adding silk powder for reaction for 1.5-2.5 hours; the components of the Ajisawa reagent are as follows: CaCl2、C2H5OH and H2The molar ratio of O is 1: (1-3): (6-10); the centrifugation conditions were: (7000-9000) rmp centrifugation for 8-12 min; the dialysis is carried out in deionized water, the cut-off value of a dialysis membrane is 5kDa, and the dialysis is carried out for 2-3 days.
5. The method for preparing the latex emulsion adhesive according to any one of claims 1 to 4, comprising the steps of:
preparing a toughening agent regenerated silk fibroin solution, mixing natural latex and the regenerated silk fibroin solution at a constant temperature, mixing a plasticizer and a thickening agent, mixing the two mixed solutions, sequentially adding a tackifier and a defoaming agent, mixing each time or adding raw materials, stirring, adding other raw materials, and finally filtering to obtain the silk fibroin composite material.
6. The method for preparing the latex emulsion adhesive according to claim 5, wherein:
mixing the natural latex and the regenerated silk fibroin solution, and stirring for 20-30 minutes;
mixing the plasticizer and the thickening agent, and stirring for 5-10 minutes;
mixing the two mixed solutions, and stirring for 5-10 minutes;
adding the tackifier and stirring for 5-10 minutes;
adding the defoaming agent, and stirring for 2-6 minutes.
7. The method for preparing the emulsion adhesive according to claim 5, wherein the constant temperature condition is 40 to 50 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911299040.XA CN110982452B (en) | 2019-12-17 | 2019-12-17 | Latex emulsion adhesive with stable mechanical property and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911299040.XA CN110982452B (en) | 2019-12-17 | 2019-12-17 | Latex emulsion adhesive with stable mechanical property and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55125133A (en) * | 1979-03-22 | 1980-09-26 | Kanebo Ltd | Foam and production thereof |
| CN103897633A (en) * | 2014-04-14 | 2014-07-02 | 太仓环亚包装制品有限公司 | Latex type natural rubber pressure-sensitive adhesive |
| CN106750611A (en) * | 2016-11-17 | 2017-05-31 | 无锡市长安曙光手套厂 | A kind of modified natural emulsion material |
| CN109749662A (en) * | 2018-12-21 | 2019-05-14 | 南京斯瑞奇医疗用品有限公司 | A kind of natural emulsion adhesive of storability and preparation method thereof |
| CN109777322A (en) * | 2018-12-21 | 2019-05-21 | 南京斯瑞奇医疗用品有限公司 | A method of improving natural emulsion base adhesive self-adhesion |
-
2019
- 2019-12-17 CN CN201911299040.XA patent/CN110982452B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55125133A (en) * | 1979-03-22 | 1980-09-26 | Kanebo Ltd | Foam and production thereof |
| CN103897633A (en) * | 2014-04-14 | 2014-07-02 | 太仓环亚包装制品有限公司 | Latex type natural rubber pressure-sensitive adhesive |
| CN106750611A (en) * | 2016-11-17 | 2017-05-31 | 无锡市长安曙光手套厂 | A kind of modified natural emulsion material |
| CN109749662A (en) * | 2018-12-21 | 2019-05-14 | 南京斯瑞奇医疗用品有限公司 | A kind of natural emulsion adhesive of storability and preparation method thereof |
| CN109777322A (en) * | 2018-12-21 | 2019-05-21 | 南京斯瑞奇医疗用品有限公司 | A method of improving natural emulsion base adhesive self-adhesion |
Non-Patent Citations (1)
| Title |
|---|
| 伊智峰: "天然橡胶/桑蚕丝丝素蛋白抗菌复合材料的制备、结构与性能", 《中国优秀硕士学位论文全文数据库 医药卫生科技辑》 * |
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