CN106675509A - Modification method of water resisting bone glue - Google Patents
Modification method of water resisting bone glue Download PDFInfo
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- CN106675509A CN106675509A CN201610967223.4A CN201610967223A CN106675509A CN 106675509 A CN106675509 A CN 106675509A CN 201610967223 A CN201610967223 A CN 201610967223A CN 106675509 A CN106675509 A CN 106675509A
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- osseocolla
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- granule
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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
- C09J189/00—Adhesives based on proteins; Adhesives based on derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H1/00—Macromolecular products derived from proteins
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Abstract
The invention discloses a modification method of water resisting bone glue. The modification method comprise the following steps of 1) mixing a bone glue particle and water at the mass ratio of 1.0:(1.5-2) at the room temperature, soaking for 12-24 hours, stirring for 20 minutes to 60 minutes at 60 DEG C to 65 DEG C after the mixture is completely swelled, then adding an acid, raising the temperature, stirring, and hydrolyzing to obtain a bone glue solution; or mixing the bone glue particle and water at the mass ratio of 1.0:(1.5-2) at the room temperature, heating to 50 DEG C to 60 DEG C, stirring for 60 minutes, dissolving to obtain a yellow transparent glue solution, then adding an acid, raising the temperature, stirring, and hydrolyzing to obtain the bone glue solution; and 2) adding sodium carboxymethylcellulose in the prepared bone glue solution, stirring to react for 60 minutes to 180 minutes, adding an organosilicon coupling agent KH560 and a paranitrophenol ethanol solution, and stirring at the constant temperature to obtain the water resisting bone glue. By the modification method, the glue, which is in a liquid state at the normal temperature, is prepared, the water resistance is improved, and the bonding mechanism of a copolymerization adhesive is studied to serve for industrialization.
Description
Technical field：
The invention belongs to polymeric material field, more particularly to a kind of water-fast using silane coupler KH560 Modify bone glues
The method of performance.
Background technology：
In recent years, the application of environmental-protection type adhesive is impregnated into the every field of national economy, and osseocolla is used as a kind of degradable
Natural glue, because bond performance is good, intensity is high, cheap, easy to use, cohering and pasting in bound book capsule
Obtain good effect.But due to its water solublity so as to which development is greatly limited.
The content of the invention：
It is an object of the invention to provide a kind of method of modifying of resistance to water osseocolla, the method is with industrial osseocolla as substantially former
Material, on the method for modifying such as original graft copolymerization basis, adds the silane coupler KH560 of hydrolyzable self-crosslinking, its molecule
In epoxy radicals and carboxyl reaction, so as to prepare enhanced water resistance energy, environmental protection green novel adhesive.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that to realize：
A kind of method of modifying of resistance to water osseocolla, comprises the following steps：
1) osseocolla granule and water are pressed into 1.0 under room temperature:(1.5-2) mass ratio mixing, soaks 12~24h, treats completely molten
After swollen, 20min-60min is stirred under the conditions of 60 DEG C -65 DEG C, be subsequently adding acid intensification stirring hydrolysis, obtain osseocolla solution；
2) in the osseocolla solution for preparing, sodium carboxymethyl cellulose or sodium lauryl sulphate or chitin are added：Carboxylic
Sodium carboxymethylcellulose pyce different proportion stirring reaction 60min-180min, then add KH560 organo silane coupling agents, to nitro
The stirring of phenol ethanol solution constant temperature obtains resistance to water osseocolla.
The present invention be further improved by, step 1) in acid used be hydrochloric acid, citric acid or sulphuric acid.
The present invention be further improved by, step 1) in hydrolysis mixing time be 30min-35min.
The present invention is further improved by, step 2) in the quality of sodium carboxymethyl cellulose that adds account for osseocolla granule matter
The 2%-4% of amount, the KH560 organo silane coupling agents of addition account for the 2%-6% of osseocolla granular mass, the paranitrophenol second of addition
Alcoholic solution accounts for the 2%-8% of the dry glue quality of osseocolla granule.
The present invention be further improved by, step 2) in constant temperature mixing time be 30min-65min.
A kind of method of modifying of resistance to water osseocolla, comprises the following steps：
1) at room temperature by osseocolla granule and water by 1.0:(1.5-2) mass ratio mixing, is heated to 50 DEG C of -60 DEG C of stirrings
35min dissolvings obtain the bright glue of yellow, are subsequently adding acid intensification stirring hydrolysis, obtain osseocolla solution；
2) in the osseocolla solution for preparing, sodium carboxymethyl cellulose or sodium lauryl sulphate or chitin are added：Carboxylic
Sodium carboxymethylcellulose pyce different proportion stirring reaction 60min-180min, then add KH560 organo silane coupling agents, to nitro
The stirring of phenol ethanol solution constant temperature obtains resistance to water Bone glue adhesive.
The present invention be further improved by, step 1) in acid used be hydrochloric acid, citric acid or sulphuric acid.
The present invention be further improved by, step 1) in hydrolysis mixing time be 30min-35min.
The present invention is further improved by, step 2) in the quality of sodium carboxymethyl cellulose that adds account for osseocolla granule matter
The 2%-4% of amount, the KH560 organo silane coupling agents of addition account for the 2%-6% of osseocolla granular mass, the paranitrophenol second of addition
Alcoholic solution accounts for the 2%-8% of the dry glue quality of osseocolla granule.
The present invention be further improved by, step 2) in constant temperature mixing time be 30min-65min.
The invention has the advantages that：
The preparation method of Bone glue adhesive of the present invention is disconnected during Bone glue adhesive is prepared using acidolysis
Peptide bond, discharges the osseocolla molecule of suitable size, then the method with KH560 silane coupler crosslinking copolymerizations, and traditional osseocolla is entered
Row is modified, and the epoxy radicals in silane coupled agent molecule occur chemical reaction with the carboxyl in osseocolla, form more linear structures,
On the one hand degree of closure of the three-dimensional-structure to methylol is reduced, the water resistance for making Modify bone glue is improved；On the other hand
Increase osseocolla strand, caking ability strengthens.Sodium carboxymethyl cellulose, paranitrophenol ethanol solution are added simultaneously to osseocolla solution
Carry out freeze proof, anti-mildew.It is at normal temperatures the adhesive of liquid that the present invention has been prepared a kind of, improves water resistance, and studies it
The bonding mechanism of copolymerization stick, is industrialization service.
Further, osseocolla contains-NH3With-COOH isoreactivity groups, mutually associate in aqueous, constitute a net
Shape insoluble solid dot matrix forms gel, and its gel state is broken at normal temperatures, can hydrolyze in acid condition, disconnects titanium
It is strong, discharge appropriately sized osseocolla molecule.Will not cause the phenomenon such as osseocolla degeneration and working life shortening using acidolysis.
Further, the acidolysis time viscosity and freezing point of Modify bone glue are had an impact, with constantly prolonging for acidolysis time
Long, in situation of falling after rising, osseocolla freezing point is in first to drop to rise situation afterwards to osseocolla viscosity, when the acidolysis time being 30min-35min,
Osseocolla freezing point is relatively minimum and viscosity is with respect to highest.
Further, sodium carboxymethyl cellulose has excellent freezing plateau, and adding can improve in Modify bone glue solution
Its freezing point.But he is a kind of water miscible sodium salt, so the amount for adding is suitable, the resistance to water of Modify bone glue is otherwise reduced.
Substantial amounts of methylol is generated during KH560 organo silane coupling agent graft copolymerizations, he has interior crosslinking feature, if content in system
It is too high, in the possibility that polymerization stage can occur to be gelled, so the 2%-6% that the quality for adding accounts for osseocolla granular mass is advisable.Bone
Glue is a kind of protein adhesive, is easily gone mouldy, and is difficult storage.And paranitrophenol has excellent anti-fungi performance, it is soluble in
In ethanol solution, and ethanol is as a kind of organic solvent, and its hydrophobic group can immerse bone glue protein intramolecule, destroy it
Molecular structure, and make its resistance to water amino acid residue fully come out.If the paranitrophenol amount amount for adding does not have very little anti-
Mould effect, water resistance too many and that ethanol can be affected, so optimised quantity is 2%-8%.
Further, on the premise of ensureing that other conditions are constant, modification time is only changed, with prolonging for modification time
Long, the time of coming unglued, between 30min-65min, the time of coming unglued was relatively most long, thus explanation long-time in trend short after first growing
Being modified can not maintain the resistance to water of Bone glue adhesive.
Additionally, the contact angle of the resistance to water osseocolla prepared according to testing result, the present invention is 113.5 °, relative to common bone
63.8 ° of the contact angle of glue, the osseocolla resistance to water for showing present invention preparation is remarkably reinforced.
Description of the drawings：
Fig. 1 is the testing result of common osseocolla contact angle, and contact angle is 63.8 °.
Fig. 2 is the testing result of resistance to water osseocolla prepared by the embodiment of the present invention 4, and contact angle is 113.5 °.
Specific embodiment：
The present invention is made further instructions with reference to embodiments.
Embodiment 1：
Osseocolla granule is mixed with cold water by 1: 1.5 mass ratio and is placed in there-necked flask, soak 12~24h, treated completely
After swelling, 65 DEG C of heating in water bath intensification, constant temperature stirring 20min, dissolving obtains osseocolla solution.At being subsequently adding hydrochloric acid, 65-70 DEG C
Hydrolysis 30min obtains the bright mucus of yellow, and temperature adds sodium carboxymethyl cellulose, isothermal reaction 90min to add when being down to 40 DEG C
Yellowish-brown thick liquid is obtained after KH560 organo silane coupling agents, paranitrophenol ethanol solution constant temperature stirring reaction 40min；Its
The hydrochloric acid of middle addition accounts for the 1% of the dry glue quality of osseocolla granule, and the sodium carboxymethyl cellulose of addition accounts for the dry glue matter of osseocolla granule
The 3% of amount, the KH560 organo silane coupling agents of addition account for the 3% of the dry glue quality of osseocolla granule, the paranitrophenol solution of addition
Account for osseocolla granule dry glue quality 5%.
Embodiment 2：
Osseocolla granule is mixed with cold water by 1: 2 mass ratio and is placed in there-necked flask, soak 12~24h, treat completely molten
After swollen, 60 DEG C of heating in water bath intensification, constant temperature stirring 35min, dissolving obtains osseocolla solution.At being subsequently adding citric acid, 65-70 DEG C
Hydrolysis 180min obtains the bright mucus of yellow, and temperature adds sodium carboxymethyl cellulose, constant temperature stirring reaction when being down to 35 DEG C
80min, to add and obtain yellowish-brown viscous solution after KH560 organo silane coupling agents, paranitrophenol solution constant temperature stirring reaction 30min
Body；The citric acid for wherein adding accounts for the 3% of the dry glue quality of osseocolla granule, and the sodium carboxymethyl cellulose of addition accounts for osseocolla granule
The 2% of dry glue quality, the KH560 organo silane coupling agents of addition account for the 2% of the dry glue quality of osseocolla granule, addition to nitro
Phenol ethanol solution accounts for the 8% of the dry glue quality of osseocolla granule.
Embodiment 3：
Osseocolla granule is mixed with water by 1: 1.5 mass ratio and is placed in there-necked flask, heating in water bath intensification 70 DEG C, constant temperature
Stirring 40min, dissolving obtains osseocolla solution.Sulphuric acid is subsequently adding, 60min is hydrolyzed at 50 DEG C and is obtained the bright mucus of yellow, while
Sodium carboxymethyl cellulose is added, 70min is reacted, KH560 organo silane coupling agents, paranitrophenol solution constant temperature stirring reaction is added
Yellowish-brown thick liquid is obtained after 60min；The sulphuric acid for wherein adding accounts for the 1.5% of the dry glue quality of osseocolla granule, the carboxylic of addition
Sodium carboxymethylcellulose pyce accounts for the 4% of the dry glue quality of osseocolla granule, and the KH560 organo silane coupling agents of addition account for the dry of osseocolla granule
Colloid amount 2.5%, the paranitrophenol ethanol solution of addition accounts for the 6% of the dry glue quality of osseocolla granule.
Embodiment 4：
Osseocolla granule is mixed with water by 1: 2 mass ratio and is placed in there-necked flask, 55 DEG C of heating in water bath intensification, constant temperature are stirred
35min is mixed, dissolving obtains osseocolla solution.Citric acid is subsequently adding, 60min is hydrolyzed at 60 DEG C and is obtained the bright mucus of yellow, while
Sodium carboxymethyl cellulose is added, 65min is reacted, KH560 organo silane coupling agents, paranitrophenol solution constant temperature stirring reaction is added
Yellowish-brown thick liquid is obtained after 60min；The citric acid for wherein adding accounts for the 1.5% of the dry glue quality of osseocolla granule, addition
Sodium carboxymethyl cellulose accounts for the 4% of the dry glue quality of osseocolla granule, and the KH560 organo silane coupling agents of addition account for osseocolla granule
Dry glue quality 6%, the paranitrophenol ethanol solution of addition accounts for the 2% of the dry glue quality of osseocolla granule.
As depicted in figs. 1 and 2, according to testing result, the contact angle of resistance to water osseocolla prepared by the present invention is 113.5 °, phase
For 63.8 ° of the contact angle of common osseocolla, the osseocolla resistance to water for showing present invention preparation is remarkably reinforced.
Embodiment 5：
Osseocolla granule is mixed with water by 1: 1.2 mass ratio and is placed in there-necked flask, heating in water bath intensification 65 DEG C, constant temperature
Stirring 40min, dissolving obtains osseocolla solution.Citric acid is subsequently adding, 35min is hydrolyzed at 65 DEG C and is obtained the bright mucus of yellow, together
When add sodium lauryl sulphate, react 60min, add KH560 organo silane coupling agents, the stirring of paranitrophenol solution constant temperature anti-
Answer and obtain after 60min yellowish-brown thick liquid；The citric acid for wherein adding accounts for the 1.5% of the dry glue quality of osseocolla granule, adds
Sodium lauryl sulphate account for osseocolla granule dry glue quality 4%, the KH560 organo silane coupling agents of addition account for osseocolla granule
Dry glue quality 6%, the paranitrophenol ethanol solution of addition accounts for the 2% of the dry glue quality of osseocolla granule.
Embodiment 6：
Osseocolla granule is mixed with water by 1: 1.2 mass ratio and is placed in there-necked flask, heating in water bath intensification 55 DEG C, constant temperature
Stirring 30min, dissolving obtains osseocolla solution.Citric acid is subsequently adding, 35min is hydrolyzed at 65 DEG C and is obtained the bright mucus of yellow, together
When add chitin：Sodium carboxymethyl cellulose mass ratio is 1:4~6, reaction 30min, addition KH560 organo silane coupling agents,
Yellowish-brown thick liquid is obtained after paranitrophenol solution constant temperature stirring reaction 65min；The citric acid for wherein adding accounts for osseocolla granule
Dry glue quality 2%, the chitin of addition：Sodium carboxymethyl cellulose accounts for the 5% of the dry glue quality of osseocolla granule, addition
KH560 organo silane coupling agents account for the dry glue quality 4% of osseocolla granule, and the paranitrophenol ethanol solution of addition accounts for osseocolla granule
The 1.5% of dry glue quality.
Claims (10)
1. a kind of method of modifying of resistance to water osseocolla, it is characterised in that comprise the following steps：
1) osseocolla granule and water are pressed into 1.0 under room temperature:(1.5-2) mass ratio mixing, soaks 12~24h, after complete swelling,
20min-60min is stirred under the conditions of 60 DEG C -65 DEG C, acid intensification stirring hydrolysis is subsequently adding, osseocolla solution is obtained；
2) in the osseocolla solution for preparing, sodium carboxymethyl cellulose or sodium lauryl sulphate or chitin are added：Carboxymethyl
Sodium cellulosate different proportion stirring reaction 60min-180min, is then adding KH560 organo silane coupling agents, paranitrophenol second
The stirring of alcoholic solution constant temperature obtains resistance to water osseocolla.
2. a kind of method of modifying of resistance to water osseocolla according to claim 1, it is characterised in that step 1) in it is used
Acid is hydrochloric acid, citric acid or sulphuric acid.
3. a kind of method of modifying of resistance to water osseocolla according to claim 1, it is characterised in that step 1) in hydrolysis stir
The time is mixed for 30min-35min.
4. a kind of method of modifying of resistance to water osseocolla according to claim 1, it is characterised in that step 2) in the carboxylic that adds
The quality of sodium carboxymethylcellulose pyce accounts for the 2%-4% of osseocolla granular mass, and the KH560 organo silane coupling agents of addition account for osseocolla granule
The 2%-6% of quality, the paranitrophenol ethanol solution of addition accounts for the 2%-8% of the dry glue quality of osseocolla granule.
5. a kind of method of modifying of resistance to water osseocolla according to claim 1, it is characterised in that step 2) in constant temperature stir
The time is mixed for 30min-65min.
6. a kind of method of modifying of resistance to water osseocolla, it is characterised in that comprise the following steps：
1) at room temperature by osseocolla granule and water by 1.0:(1.5-2) mass ratio mixing, is heated to 50 DEG C of -60 DEG C of stirrings
35min dissolvings obtain the bright glue of yellow, are subsequently adding acid intensification stirring hydrolysis, obtain osseocolla solution；
2) in the osseocolla solution for preparing, sodium carboxymethyl cellulose or sodium lauryl sulphate or chitin are added：Carboxymethyl
Sodium cellulosate different proportion stirring reaction 60min-180min, is then adding KH560 organo silane coupling agents, paranitrophenol second
The stirring of alcoholic solution constant temperature obtains resistance to water Bone glue adhesive.
7. a kind of method of modifying of resistance to water osseocolla according to claim 6, it is characterised in that step 1) in it is used
Acid is hydrochloric acid, citric acid or sulphuric acid.
8. a kind of method of modifying of resistance to water osseocolla according to claim 6, it is characterised in that step 1) in hydrolysis stir
The time is mixed for 30min-35min.
9. a kind of method of modifying of resistance to water osseocolla according to claim 6, it is characterised in that step 2) in the carboxylic that adds
The quality of sodium carboxymethylcellulose pyce accounts for the 2%-4% of osseocolla granular mass, and the KH560 organo silane coupling agents of addition account for osseocolla granule
The 2%-6% of quality, the paranitrophenol ethanol solution of addition accounts for the 2%-8% of the dry glue quality of osseocolla granule.
10. a kind of method of modifying of resistance to water osseocolla according to claim 6, it is characterised in that step 2) in constant temperature
Mixing time is 30min-65min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610967223.4A CN106675509B (en) | 2016-10-28 | 2016-10-28 | A kind of method of modifying of water resistance gelatine |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610967223.4A CN106675509B (en) | 2016-10-28 | 2016-10-28 | A kind of method of modifying of water resistance gelatine |
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| CN106675509B CN106675509B (en) | 2019-04-02 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516762A (en) * | 2018-04-25 | 2018-09-11 | 江苏新亿源环保科技有限公司 | A kind of permanent seal cooling anti-strip vitrified bonding |
| CN109485456A (en) * | 2019-01-08 | 2019-03-19 | 陈爱民 | A kind of foam concrete light partition board and its production technology |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627944A (en) * | 2012-04-12 | 2012-08-08 | 陕西科技大学 | Modified bone glue adhesive and preparation method thereof |
| CN103525360A (en) * | 2013-09-26 | 2014-01-22 | 陕西科技大学 | Preparation method of hydrophobic bone glue |
| CN104610908A (en) * | 2015-01-16 | 2015-05-13 | 陕西科技大学 | Liquid bone glue adhesive modification method |
-
2016
- 2016-10-28 CN CN201610967223.4A patent/CN106675509B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627944A (en) * | 2012-04-12 | 2012-08-08 | 陕西科技大学 | Modified bone glue adhesive and preparation method thereof |
| CN103525360A (en) * | 2013-09-26 | 2014-01-22 | 陕西科技大学 | Preparation method of hydrophobic bone glue |
| CN104610908A (en) * | 2015-01-16 | 2015-05-13 | 陕西科技大学 | Liquid bone glue adhesive modification method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516762A (en) * | 2018-04-25 | 2018-09-11 | 江苏新亿源环保科技有限公司 | A kind of permanent seal cooling anti-strip vitrified bonding |
| CN109485456A (en) * | 2019-01-08 | 2019-03-19 | 陈爱民 | A kind of foam concrete light partition board and its production technology |
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| Publication number | Publication date |
|---|---|
| CN106675509B (en) | 2019-04-02 |
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